Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Christoph Janiak' 'Friedrich Drepper' 'Wolfgang Haehnel' 'Wen-Hua Sun' 'Biao Wu' 'Xiao-Juan Yang' _publ_contact_author_name 'ProfD Christoph Janiak' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Univ. Freiburg Albertstr. 21 Freiburg 79104 GERMANY ; _publ_contact_author_email JANIAK@UNI-FREIBURG.DE _publ_requested_journal 'Dalton Transactions' _publ_section_title ; >From model compounds to protein binding: Syntheses, characterizations and fluorescence studies of [RuII(bipy)(terpy)L]2+ complexes (bipy = 2,2'-bipyridine; terpy = 2,2':6',2''-terpyridine; L = imidazole, pyrazole and derivatives, cytochrome c, plastocyanin) ; data_ruo _database_code_depnum_ccdc_archive 'CCDC 251479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Aqua(2,2'-bipyridine)(2,2':6',2''-terpyridine)- ruthenium(II)]bis(hexafluorophosphate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(H2 O)(C10 H8 N2)(C15 H11 N3)Ru](P F6)2' _chemical_formula_sum 'C25 H21 F12 N5 O P2 Ru' _chemical_formula_weight 798.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinc _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.976(10) _cell_length_b 10.567(6) _cell_length_c 15.275(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.938(12) _cell_angle_gamma 90.00 _cell_volume 2726(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8550 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10966 _diffrn_reflns_av_R_equivalents 0.1047 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4818 _reflns_number_gt 3559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms on carbon were calculated using appropriate riding models (AFIX 43, U(H) = 1.2 Ueq(C). Hydrogen atoms of aqua ligand were located in the difference map and refined by restraining the O-H bond lengths to 0.9+/-0.05 Ang together with isotropic displacement parameters (Ueq = 1.2 Ueq(O)). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+30.7413P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4818 _refine_ls_number_parameters 466 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.73700(3) 0.21601(6) 0.69980(4) 0.03834(19) Uani 1 1 d . . . O O 0.6355(3) 0.1913(6) 0.7654(4) 0.0512(14) Uani 1 1 d D . . H1 H 0.610(5) 0.122(6) 0.759(6) 0.061 Uiso 1 1 d D . . H2 H 0.602(4) 0.258(6) 0.769(6) 0.061 Uiso 1 1 d D . . N1 N 0.7651(4) 0.3682(6) 0.7757(4) 0.0462(15) Uani 1 1 d . . . N2 N 0.6835(3) 0.3440(6) 0.6282(4) 0.0421(14) Uani 1 1 d . . . N3 N 0.6886(3) 0.1112(6) 0.5974(4) 0.0397(14) Uani 1 1 d . . . N4 N 0.8385(3) 0.2186(6) 0.6482(4) 0.0425(14) Uani 1 1 d . . . N5 N 0.7980(3) 0.0904(6) 0.7767(4) 0.0392(13) Uani 1 1 d . . . C1 C 0.8073(5) 0.3731(9) 0.8510(5) 0.055(2) Uani 1 1 d . . . H1A H 0.8286 0.2987 0.8760 0.066 Uiso 1 1 calc R . . C2 C 0.8214(6) 0.4833(10) 0.8943(6) 0.071(3) Uani 1 1 d . . . H2A H 0.8536 0.4847 0.9474 0.085 Uiso 1 1 calc R . . C3 C 0.7891(6) 0.5902(9) 0.8612(6) 0.069(3) Uani 1 1 d . . . H3A H 0.7972 0.6661 0.8915 0.083 Uiso 1 1 calc R . . C4 C 0.7458(5) 0.5863(8) 0.7848(6) 0.056(2) Uani 1 1 d . . . H4A H 0.7240 0.6605 0.7601 0.067 Uiso 1 1 calc R . . C5 C 0.7328(5) 0.4758(7) 0.7421(5) 0.0461(18) Uani 1 1 d . . . C6 C 0.6872(4) 0.4615(8) 0.6578(5) 0.0450(18) Uani 1 1 d . . . C7 C 0.6484(5) 0.5534(8) 0.6088(6) 0.060(2) Uani 1 1 d . . . H7A H 0.6495 0.6367 0.6285 0.072 Uiso 1 1 calc R . . C8 C 0.6093(6) 0.5230(10) 0.5331(6) 0.068(3) Uani 1 1 d . . . H8A H 0.5844 0.5862 0.4981 0.082 Uiso 1 1 calc R . . C9 C 0.6046(5) 0.4020(10) 0.5048(6) 0.061(2) Uani 1 1 d . . . H9A H 0.5753 0.3815 0.4519 0.073 Uiso 1 1 calc R . . C10 C 0.6425(4) 0.3126(8) 0.5540(5) 0.0465(18) Uani 1 1 d . . . C11 C 0.6446(5) 0.1793(8) 0.5374(5) 0.050(2) Uani 1 1 d . . . C12 C 0.6058(6) 0.1242(11) 0.4667(6) 0.070(3) Uani 1 1 d . . . H12A H 0.5750 0.1725 0.4253 0.084 Uiso 1 1 calc R . . C13 C 0.6118(6) -0.0019(11) 0.4562(7) 0.076(3) Uani 1 1 d . . . H13A H 0.5845 -0.0418 0.4080 0.091 Uiso 1 1 calc R . . C14 C 0.6571(6) -0.0685(10) 0.5153(6) 0.067(2) Uani 1 1 d . . . H14A H 0.6627 -0.1554 0.5082 0.081 Uiso 1 1 calc R . . C15 C 0.6939(5) -0.0112(8) 0.5836(6) 0.053(2) Uani 1 1 d . . . H15A H 0.7255 -0.0593 0.6244 0.064 Uiso 1 1 calc R . . C16 C 0.8542(5) 0.2835(9) 0.5800(5) 0.054(2) Uani 1 1 d . . . H16A H 0.8175 0.3432 0.5568 0.065 Uiso 1 1 calc R . . C17 C 0.9209(5) 0.2685(10) 0.5416(6) 0.062(2) Uani 1 1 d . . . H17A H 0.9298 0.3160 0.4923 0.074 Uiso 1 1 calc R . . C18 C 0.9740(6) 0.1855(10) 0.5745(6) 0.069(3) Uani 1 1 d . . . H18A H 1.0203 0.1727 0.5481 0.083 Uiso 1 1 calc R . . C19 C 0.9604(5) 0.1208(9) 0.6455(6) 0.062(2) Uani 1 1 d . . . H19A H 0.9978 0.0629 0.6697 0.074 Uiso 1 1 calc R . . C20 C 0.8928(4) 0.1380(7) 0.6830(5) 0.0430(17) Uani 1 1 d . . . C21 C 0.8719(4) 0.0731(7) 0.7591(5) 0.0416(16) Uani 1 1 d . . . C22 C 0.9228(5) 0.0036(8) 0.8122(6) 0.061(2) Uani 1 1 d . . . H22A H 0.9750 -0.0059 0.7997 0.073 Uiso 1 1 calc R . . C23 C 0.8984(6) -0.0517(9) 0.8827(6) 0.072(3) Uani 1 1 d . . . H23A H 0.9331 -0.0992 0.9207 0.086 Uiso 1 1 calc R . . C24 C 0.8224(6) -0.0372(9) 0.8978(6) 0.064(2) Uani 1 1 d . . . H24A H 0.8035 -0.0770 0.9457 0.076 Uiso 1 1 calc R . . C25 C 0.7751(5) 0.0326(7) 0.8454(5) 0.0472(18) Uani 1 1 d . . . H25A H 0.7228 0.0417 0.8573 0.057 Uiso 1 1 calc R . . P1 P 0.44783(16) 0.1444(3) 0.2301(2) 0.0775(8) Uani 1 1 d D . . F1 F 0.5363(3) 0.1142(7) 0.2543(6) 0.112(2) Uani 1 1 d D A . F2 F 0.4659(16) 0.2237(16) 0.3150(9) 0.107(7) Uani 0.50 1 d PD A 1 F4 F 0.3621(5) 0.1588(12) 0.2510(11) 0.106(4) Uani 0.60 1 d PD A 1 F6 F 0.4954(17) 0.196(3) 0.1560(19) 0.128(12) Uani 0.40 1 d PD A 1 F4' F 0.3730(10) 0.184(2) 0.1620(15) 0.184(8) Uani 0.60 1 d P A 2 F2' F 0.4541(19) 0.281(3) 0.263(3) 0.176(18) Uani 0.40 1 d P A 2 F6' F 0.4618(17) 0.244(2) 0.1710(18) 0.140(11) Uani 0.50 1 d P A 2 F3 F 0.4382(6) 0.0400(9) 0.3015(6) 0.160(4) Uani 1 1 d D A . F5 F 0.4397(5) 0.0330(7) 0.1679(5) 0.132(3) Uani 1 1 d D A . P2 P 0.11435(14) 0.2311(3) 0.87470(14) 0.0611(6) Uani 1 1 d D . . F7 F 0.1958(7) 0.200(2) 0.9205(15) 0.143(8) Uani 0.60 1 d PD B 1 F8 F 0.1165(11) 0.3662(12) 0.9158(14) 0.097(6) Uani 0.40 1 d PD B 1 F7' F 0.1731(15) 0.126(2) 0.8968(14) 0.138(10) Uani 0.50 1 d P B 2 F8' F 0.1300(9) 0.2848(18) 0.9640(9) 0.100(5) Uani 0.50 1 d P B 2 F9 F 0.0619(5) 0.1557(9) 0.9315(5) 0.138(3) Uani 1 1 d D B . F10 F 0.0375(4) 0.2885(10) 0.8380(7) 0.159(4) Uani 1 1 d D B . F11 F 0.1013(6) 0.1313(10) 0.8037(7) 0.170(5) Uani 1 1 d D B . F12 F 0.1663(5) 0.2992(7) 0.8148(5) 0.124(3) Uani 1 1 d D B . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0396(3) 0.0394(3) 0.0356(3) 0.0072(3) 0.0016(2) 0.0016(3) O 0.043(3) 0.054(3) 0.059(3) 0.009(3) 0.015(3) 0.002(3) N1 0.051(4) 0.047(4) 0.040(3) -0.001(3) 0.004(3) -0.004(3) N2 0.033(3) 0.046(4) 0.047(4) 0.010(3) 0.005(3) 0.002(3) N3 0.037(3) 0.042(3) 0.040(3) 0.003(3) 0.003(2) -0.003(3) N4 0.044(3) 0.046(3) 0.035(3) 0.007(3) -0.003(2) -0.009(3) N5 0.040(3) 0.040(3) 0.037(3) 0.007(3) -0.005(2) -0.001(3) C1 0.062(5) 0.056(5) 0.046(5) -0.002(4) -0.002(4) -0.003(4) C2 0.077(7) 0.077(7) 0.057(6) -0.009(5) -0.004(5) -0.009(6) C3 0.095(7) 0.053(5) 0.061(6) -0.015(5) 0.013(5) -0.014(5) C4 0.067(6) 0.041(4) 0.063(6) 0.002(4) 0.019(4) -0.001(4) C5 0.049(5) 0.045(4) 0.045(4) 0.013(4) 0.008(3) 0.003(4) C6 0.041(4) 0.047(4) 0.047(4) 0.006(4) 0.008(3) -0.002(4) C7 0.071(6) 0.044(5) 0.066(6) 0.021(4) 0.012(5) 0.016(4) C8 0.068(6) 0.078(7) 0.059(6) 0.031(5) 0.000(4) 0.022(5) C9 0.064(6) 0.075(6) 0.043(5) 0.012(5) 0.001(4) 0.005(5) C10 0.048(4) 0.060(5) 0.031(4) 0.006(4) 0.001(3) 0.002(4) C11 0.047(4) 0.064(5) 0.040(4) 0.003(4) 0.007(3) -0.010(4) C12 0.070(6) 0.092(8) 0.046(5) -0.004(5) -0.003(4) -0.003(6) C13 0.086(7) 0.083(7) 0.058(6) -0.027(6) 0.007(5) -0.024(6) C14 0.083(7) 0.059(6) 0.060(6) -0.010(5) 0.010(5) -0.002(5) C15 0.057(5) 0.050(5) 0.055(5) -0.011(4) 0.017(4) -0.007(4) C16 0.049(5) 0.060(5) 0.053(5) 0.020(4) 0.004(4) -0.002(4) C17 0.047(5) 0.081(6) 0.059(5) 0.018(5) 0.010(4) -0.015(5) C18 0.056(5) 0.084(7) 0.070(6) 0.005(6) 0.022(5) -0.011(5) C19 0.043(5) 0.069(6) 0.073(6) 0.011(5) 0.006(4) 0.004(4) C20 0.037(4) 0.040(4) 0.051(4) 0.003(4) 0.002(3) -0.002(3) C21 0.045(4) 0.036(4) 0.043(4) 0.003(3) -0.003(3) 0.001(3) C22 0.057(5) 0.055(5) 0.069(6) 0.017(5) -0.002(4) 0.017(4) C23 0.081(7) 0.065(6) 0.064(6) 0.024(5) -0.012(5) 0.019(6) C24 0.082(7) 0.060(5) 0.048(5) 0.021(4) 0.003(4) -0.001(5) C25 0.058(5) 0.041(4) 0.041(4) 0.015(4) 0.001(3) 0.005(4) P1 0.0633(17) 0.0683(17) 0.102(2) -0.0274(16) 0.0166(15) -0.0193(15) F1 0.086(5) 0.095(5) 0.154(7) 0.003(5) 0.002(4) -0.017(4) F2 0.116(13) 0.080(13) 0.123(13) -0.051(10) 0.002(11) 0.003(12) F4 0.062(6) 0.091(8) 0.167(12) -0.005(9) 0.017(7) 0.007(6) F6 0.084(18) 0.15(3) 0.16(2) 0.01(2) 0.046(18) -0.033(17) F4' 0.106(12) 0.191(19) 0.25(2) -0.046(19) -0.018(13) 0.034(13) F2' 0.12(2) 0.09(2) 0.34(4) -0.15(3) 0.11(3) -0.049(18) F6' 0.15(3) 0.084(15) 0.17(3) 0.090(19) -0.043(15) -0.016(14) F3 0.190(9) 0.161(8) 0.140(7) -0.003(7) 0.071(7) -0.069(8) F5 0.182(8) 0.103(6) 0.104(6) -0.043(5) -0.019(5) -0.025(6) P2 0.0663(15) 0.0750(16) 0.0430(12) 0.0013(12) 0.0105(10) 0.0048(14) F7 0.082(9) 0.158(18) 0.181(19) 0.062(16) -0.019(10) 0.026(12) F8 0.106(13) 0.065(10) 0.121(16) -0.055(10) 0.016(12) 0.005(10) F7' 0.20(2) 0.128(18) 0.104(14) 0.035(13) 0.079(15) 0.071(16) F8' 0.097(10) 0.132(13) 0.071(9) -0.058(9) 0.008(7) -0.021(11) F9 0.137(6) 0.181(8) 0.107(6) 0.036(6) 0.063(5) -0.007(6) F10 0.097(6) 0.168(9) 0.208(10) 0.054(8) 0.007(6) 0.046(6) F11 0.152(8) 0.199(10) 0.171(9) -0.106(8) 0.081(7) -0.077(8) F12 0.133(6) 0.109(6) 0.137(6) 0.019(5) 0.050(5) -0.032(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 1.909(6) . ? Ru N4 1.969(6) . ? Ru N5 1.991(6) . ? Ru N1 2.010(6) . ? Ru N3 2.020(6) . ? Ru O 2.097(5) . ? O H1 0.85(5) . ? O H2 0.92(5) . ? N1 C1 1.293(10) . ? N1 C5 1.340(10) . ? N2 C10 1.311(9) . ? N2 C6 1.320(10) . ? N3 C15 1.315(10) . ? N3 C11 1.332(10) . ? N4 C16 1.298(9) . ? N4 C20 1.325(9) . ? N5 C25 1.308(9) . ? N5 C21 1.322(9) . ? C1 C2 1.348(13) . ? C1 H1A 0.9300 . ? C2 C3 1.332(14) . ? C2 H2A 0.9300 . ? C3 C4 1.314(13) . ? C3 H3A 0.9300 . ? C4 C5 1.344(11) . ? C4 H4A 0.9300 . ? C5 C6 1.441(11) . ? C6 C7 1.354(11) . ? C7 C8 1.313(13) . ? C7 H7A 0.9300 . ? C8 C9 1.349(14) . ? C8 H8A 0.9300 . ? C9 C10 1.330(11) . ? C9 H9A 0.9300 . ? C10 C11 1.433(12) . ? C11 C12 1.337(12) . ? C12 C13 1.348(15) . ? C12 H12A 0.9300 . ? C13 C14 1.326(14) . ? C13 H13A 0.9300 . ? C14 C15 1.308(12) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.337(11) . ? C16 H16A 0.9300 . ? C17 C18 1.319(13) . ? C17 H17A 0.9300 . ? C18 C19 1.323(12) . ? C18 H18A 0.9300 . ? C19 C20 1.347(10) . ? C19 H19A 0.9300 . ? C20 C21 1.426(10) . ? C21 C22 1.341(10) . ? C22 C23 1.329(12) . ? C22 H22A 0.9300 . ? C23 C24 1.343(13) . ? C23 H23A 0.9300 . ? C24 C25 1.302(11) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? P1 F6' 1.421(17) . ? P1 F5 1.510(6) . ? P1 F4 1.529(8) . ? P1 F2' 1.53(2) . ? P1 F1 1.542(6) . ? P1 F2 1.548(10) . ? P1 F6 1.555(10) . ? P1 F3 1.572(7) . ? P1 F4' 1.609(18) . ? F4' F6' 1.63(3) . ? F2' F6' 1.48(4) . ? P2 F8' 1.475(12) . ? P2 F10 1.494(6) . ? P2 F7' 1.51(2) . ? P2 F11 1.512(7) . ? P2 F12 1.517(6) . ? P2 F7 1.519(9) . ? P2 F9 1.529(6) . ? P2 F8 1.558(9) . ? F7' F11 1.78(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru N4 98.3(2) . . ? N2 Ru N5 176.4(3) . . ? N4 Ru N5 79.7(2) . . ? N2 Ru N1 80.4(3) . . ? N4 Ru N1 93.1(3) . . ? N5 Ru N1 96.6(3) . . ? N2 Ru N3 79.3(3) . . ? N4 Ru N3 90.0(2) . . ? N5 Ru N3 103.7(2) . . ? N1 Ru N3 159.7(3) . . ? N2 Ru O 89.8(2) . . ? N4 Ru O 171.8(2) . . ? N5 Ru O 92.2(2) . . ? N1 Ru O 89.0(2) . . ? N3 Ru O 90.7(2) . . ? Ru O H1 119(6) . . ? Ru O H2 119(5) . . ? H1 O H2 111(8) . . ? C1 N1 C5 118.3(7) . . ? C1 N1 Ru 128.4(6) . . ? C5 N1 Ru 113.3(5) . . ? C10 N2 C6 122.4(7) . . ? C10 N2 Ru 119.7(6) . . ? C6 N2 Ru 117.9(5) . . ? C15 N3 C11 117.6(7) . . ? C15 N3 Ru 129.4(6) . . ? C11 N3 Ru 113.0(5) . . ? C16 N4 C20 118.1(7) . . ? C16 N4 Ru 126.1(6) . . ? C20 N4 Ru 115.5(5) . . ? C25 N5 C21 117.8(6) . . ? C25 N5 Ru 127.2(5) . . ? C21 N5 Ru 114.8(5) . . ? N1 C1 C2 121.7(9) . . ? N1 C1 H1A 119.2 . . ? C2 C1 H1A 119.2 . . ? C3 C2 C1 120.1(9) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 118.8(9) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 120.4(9) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? N1 C5 C4 120.8(7) . . ? N1 C5 C6 114.4(7) . . ? C4 C5 C6 124.8(8) . . ? N2 C6 C7 118.9(8) . . ? N2 C6 C5 113.9(7) . . ? C7 C6 C5 127.2(8) . . ? C8 C7 C6 118.9(9) . . ? C8 C7 H7A 120.5 . . ? C6 C7 H7A 120.5 . . ? C7 C8 C9 121.5(9) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C10 C9 C8 118.9(9) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? N2 C10 C9 119.4(8) . . ? N2 C10 C11 112.4(7) . . ? C9 C10 C11 128.2(8) . . ? N3 C11 C12 121.0(9) . . ? N3 C11 C10 115.6(7) . . ? C12 C11 C10 123.5(9) . . ? C11 C12 C13 119.3(10) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C14 C13 C12 119.3(10) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C15 C14 C13 119.5(10) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 N3 123.3(9) . . ? C14 C15 H15A 118.4 . . ? N3 C15 H15A 118.4 . . ? N4 C16 C17 122.8(8) . . ? N4 C16 H16A 118.6 . . ? C17 C16 H16A 118.6 . . ? C18 C17 C16 119.2(8) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 119.0(9) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C18 C19 C20 120.6(9) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? N4 C20 C19 120.2(7) . . ? N4 C20 C21 114.6(6) . . ? C19 C20 C21 125.2(7) . . ? N5 C21 C22 121.3(7) . . ? N5 C21 C20 114.8(6) . . ? C22 C21 C20 123.9(7) . . ? C23 C22 C21 119.6(9) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C22 C23 C24 118.4(8) . . ? C22 C23 H23A 120.8 . . ? C24 C23 H23A 120.8 . . ? C25 C24 C23 120.1(8) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 N5 122.8(8) . . ? C24 C25 H25A 118.6 . . ? N5 C25 H25A 118.6 . . ? F6' P1 F5 100.9(14) . . ? F6' P1 F4 106.5(13) . . ? F5 P1 F4 100.5(6) . . ? F6' P1 F2' 60(2) . . ? F5 P1 F2' 161(2) . . ? F4 P1 F2' 82.6(12) . . ? F6' P1 F1 94.8(11) . . ? F5 P1 F1 90.7(5) . . ? F4 P1 F1 153.4(7) . . ? F2' P1 F1 94.8(14) . . ? F6' P1 F2 95.7(15) . . ? F5 P1 F2 161.1(8) . . ? F4 P1 F2 83.1(12) . . ? F2' P1 F2 37.9(19) . . ? F1 P1 F2 78.9(10) . . ? F6' P1 F6 31.3(13) . . ? F5 P1 F6 80.6(16) . . ? F4 P1 F6 134.0(13) . . ? F2' P1 F6 83.5(18) . . ? F1 P1 F6 71.4(12) . . ? F2 P1 F6 110.3(18) . . ? F6' P1 F3 174.8(13) . . ? F5 P1 F3 83.1(5) . . ? F4 P1 F3 75.8(6) . . ? F2' P1 F3 116.2(19) . . ? F1 P1 F3 81.8(5) . . ? F2 P1 F3 79.9(9) . . ? F6 P1 F3 148.2(12) . . ? F6' P1 F4' 64.7(14) . . ? F5 P1 F4' 77.3(8) . . ? F4 P1 F4' 53.5(8) . . ? F2' P1 F4' 89.7(19) . . ? F1 P1 F4' 153.1(9) . . ? F2 P1 F4' 118.4(11) . . ? F6 P1 F4' 82.8(14) . . ? F3 P1 F4' 119.8(10) . . ? P1 F4' F6' 52.1(8) . . ? F6' F2' P1 56.2(11) . . ? P1 F6' F2' 63.7(15) . . ? P1 F6' F4' 63.2(13) . . ? F2' F6' F4' 91(2) . . ? F8' P2 F10 105.0(8) . . ? F8' P2 F7' 91.4(11) . . ? F10 P2 F7' 156.1(12) . . ? F8' P2 F11 158.4(10) . . ? F10 P2 F11 87.5(6) . . ? F7' P2 F11 72.0(10) . . ? F8' P2 F12 108.3(7) . . ? F10 P2 F12 96.9(5) . . ? F7' P2 F12 94.2(9) . . ? F11 P2 F12 87.1(5) . . ? F8' P2 F7 65.6(11) . . ? F10 P2 F7 167.8(10) . . ? F7' P2 F7 35.9(11) . . ? F11 P2 F7 103.9(10) . . ? F12 P2 F7 79.7(9) . . ? F8' P2 F9 74.7(7) . . ? F10 P2 F9 83.6(5) . . ? F7' P2 F9 84.2(9) . . ? F11 P2 F9 89.6(5) . . ? F12 P2 F9 176.7(5) . . ? F7 P2 F9 100.5(9) . . ? F8' P2 F8 44.0(8) . . ? F10 P2 F8 76.3(9) . . ? F7' P2 F8 126.7(13) . . ? F11 P2 F8 157.4(10) . . ? F12 P2 F8 79.5(9) . . ? F7 P2 F8 91.6(11) . . ? F9 P2 F8 103.8(9) . . ? P2 F7' F11 54.1(8) . . ? P2 F11 F7' 53.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru N1 C1 179.9(7) . . . . ? N4 Ru N1 C1 -82.2(7) . . . . ? N5 Ru N1 C1 -2.2(7) . . . . ? N3 Ru N1 C1 179.3(7) . . . . ? O Ru N1 C1 89.9(7) . . . . ? N2 Ru N1 C5 1.7(5) . . . . ? N4 Ru N1 C5 99.6(5) . . . . ? N5 Ru N1 C5 179.6(5) . . . . ? N3 Ru N1 C5 1.1(10) . . . . ? O Ru N1 C5 -88.3(5) . . . . ? N4 Ru N2 C10 89.6(6) . . . . ? N5 Ru N2 C10 147(4) . . . . ? N1 Ru N2 C10 -178.6(6) . . . . ? N3 Ru N2 C10 1.2(5) . . . . ? O Ru N2 C10 -89.6(6) . . . . ? N4 Ru N2 C6 -92.9(6) . . . . ? N5 Ru N2 C6 -36(4) . . . . ? N1 Ru N2 C6 -1.1(5) . . . . ? N3 Ru N2 C6 178.7(6) . . . . ? O Ru N2 C6 87.9(6) . . . . ? N2 Ru N3 C15 178.9(7) . . . . ? N4 Ru N3 C15 80.4(7) . . . . ? N5 Ru N3 C15 1.0(7) . . . . ? N1 Ru N3 C15 179.5(7) . . . . ? O Ru N3 C15 -91.5(7) . . . . ? N2 Ru N3 C11 -2.1(5) . . . . ? N4 Ru N3 C11 -100.6(5) . . . . ? N5 Ru N3 C11 180.0(5) . . . . ? N1 Ru N3 C11 -1.5(10) . . . . ? O Ru N3 C11 87.5(5) . . . . ? N2 Ru N4 C16 -5.8(7) . . . . ? N5 Ru N4 C16 177.3(7) . . . . ? N1 Ru N4 C16 -86.5(7) . . . . ? N3 Ru N4 C16 73.4(7) . . . . ? O Ru N4 C16 168.8(15) . . . . ? N2 Ru N4 C20 -179.9(5) . . . . ? N5 Ru N4 C20 3.1(5) . . . . ? N1 Ru N4 C20 99.3(6) . . . . ? N3 Ru N4 C20 -100.8(5) . . . . ? O Ru N4 C20 -5(2) . . . . ? N2 Ru N5 C25 118(4) . . . . ? N4 Ru N5 C25 175.8(7) . . . . ? N1 Ru N5 C25 83.8(7) . . . . ? N3 Ru N5 C25 -96.8(7) . . . . ? O Ru N5 C25 -5.4(7) . . . . ? N2 Ru N5 C21 -56(4) . . . . ? N4 Ru N5 C21 1.6(5) . . . . ? N1 Ru N5 C21 -90.4(5) . . . . ? N3 Ru N5 C21 89.1(5) . . . . ? O Ru N5 C21 -179.6(5) . . . . ? C5 N1 C1 C2 -2.1(12) . . . . ? Ru N1 C1 C2 179.7(7) . . . . ? N1 C1 C2 C3 2.4(15) . . . . ? C1 C2 C3 C4 -2.1(15) . . . . ? C2 C3 C4 C5 1.6(15) . . . . ? C1 N1 C5 C4 1.6(11) . . . . ? Ru N1 C5 C4 -180.0(6) . . . . ? C1 N1 C5 C6 179.6(7) . . . . ? Ru N1 C5 C6 -2.0(8) . . . . ? C3 C4 C5 N1 -1.4(13) . . . . ? C3 C4 C5 C6 -179.2(8) . . . . ? C10 N2 C6 C7 -1.4(11) . . . . ? Ru N2 C6 C7 -178.8(6) . . . . ? C10 N2 C6 C5 177.7(6) . . . . ? Ru N2 C6 C5 0.3(8) . . . . ? N1 C5 C6 N2 1.1(10) . . . . ? C4 C5 C6 N2 179.0(7) . . . . ? N1 C5 C6 C7 -179.8(8) . . . . ? C4 C5 C6 C7 -2.0(13) . . . . ? N2 C6 C7 C8 -0.9(12) . . . . ? C5 C6 C7 C8 -179.8(8) . . . . ? C6 C7 C8 C9 2.6(14) . . . . ? C7 C8 C9 C10 -2.0(15) . . . . ? C6 N2 C10 C9 1.9(11) . . . . ? Ru N2 C10 C9 179.2(6) . . . . ? C6 N2 C10 C11 -177.4(7) . . . . ? Ru N2 C10 C11 -0.1(9) . . . . ? C8 C9 C10 N2 -0.2(13) . . . . ? C8 C9 C10 C11 179.0(9) . . . . ? C15 N3 C11 C12 1.5(11) . . . . ? Ru N3 C11 C12 -177.6(7) . . . . ? C15 N3 C11 C10 -178.2(7) . . . . ? Ru N3 C11 C10 2.7(8) . . . . ? N2 C10 C11 N3 -1.8(10) . . . . ? C9 C10 C11 N3 178.9(8) . . . . ? N2 C10 C11 C12 178.5(8) . . . . ? C9 C10 C11 C12 -0.7(14) . . . . ? N3 C11 C12 C13 -0.3(14) . . . . ? C10 C11 C12 C13 179.4(9) . . . . ? C11 C12 C13 C14 -1.2(16) . . . . ? C12 C13 C14 C15 1.3(16) . . . . ? C13 C14 C15 N3 0.0(14) . . . . ? C11 N3 C15 C14 -1.4(12) . . . . ? Ru N3 C15 C14 177.6(6) . . . . ? C20 N4 C16 C17 3.0(13) . . . . ? Ru N4 C16 C17 -171.1(7) . . . . ? N4 C16 C17 C18 -0.9(15) . . . . ? C16 C17 C18 C19 -1.1(15) . . . . ? C17 C18 C19 C20 0.9(15) . . . . ? C16 N4 C20 C19 -3.1(12) . . . . ? Ru N4 C20 C19 171.6(6) . . . . ? C16 N4 C20 C21 178.3(7) . . . . ? Ru N4 C20 C21 -7.0(8) . . . . ? C18 C19 C20 N4 1.2(14) . . . . ? C18 C19 C20 C21 179.6(9) . . . . ? C25 N5 C21 C22 -3.1(11) . . . . ? Ru N5 C21 C22 171.6(7) . . . . ? C25 N5 C21 C20 179.5(7) . . . . ? Ru N5 C21 C20 -5.7(8) . . . . ? N4 C20 C21 N5 8.4(10) . . . . ? C19 C20 C21 N5 -170.1(8) . . . . ? N4 C20 C21 C22 -168.9(8) . . . . ? C19 C20 C21 C22 12.6(13) . . . . ? N5 C21 C22 C23 1.6(14) . . . . ? C20 C21 C22 C23 178.7(9) . . . . ? C21 C22 C23 C24 0.9(15) . . . . ? C22 C23 C24 C25 -1.9(15) . . . . ? C23 C24 C25 N5 0.4(15) . . . . ? C21 N5 C25 C24 2.2(12) . . . . ? Ru N5 C25 C24 -171.8(7) . . . . ? F5 P1 F4' F6' -108.7(16) . . . . ? F4 P1 F4' F6' 137.8(19) . . . . ? F2' P1 F4' F6' 56.7(18) . . . . ? F1 P1 F4' F6' -43(3) . . . . ? F2 P1 F4' F6' 82.5(18) . . . . ? F6 P1 F4' F6' -27(2) . . . . ? F3 P1 F4' F6' 177.1(16) . . . . ? F5 P1 F2' F6' -13(5) . . . . ? F4 P1 F2' F6' -114(2) . . . . ? F1 P1 F2' F6' 92.7(18) . . . . ? F2 P1 F2' F6' 158(4) . . . . ? F6 P1 F2' F6' 22(2) . . . . ? F3 P1 F2' F6' 175.9(14) . . . . ? F4' P1 F2' F6' -60.7(19) . . . . ? F5 P1 F6' F2' 175.5(18) . . . . ? F4 P1 F6' F2' 71(2) . . . . ? F1 P1 F6' F2' -92.8(19) . . . . ? F2 P1 F6' F2' -13(3) . . . . ? F6 P1 F6' F2' -134(5) . . . . ? F3 P1 F6' F2' -45(16) . . . . ? F4' P1 F6' F2' 105(2) . . . . ? F5 P1 F6' F4' 70.2(11) . . . . ? F4 P1 F6' F4' -34.3(14) . . . . ? F2' P1 F6' F4' -105(2) . . . . ? F1 P1 F6' F4' 161.9(10) . . . . ? F2 P1 F6' F4' -118.8(14) . . . . ? F6 P1 F6' F4' 121(5) . . . . ? F3 P1 F6' F4' -150(14) . . . . ? P1 F2' F6' F4' 59.5(12) . . . . ? P1 F4' F6' F2' -59.9(17) . . . . ? F8' P2 F7' F11 165.9(8) . . . . ? F10 P2 F7' F11 32(2) . . . . ? F12 P2 F7' F11 -85.6(6) . . . . ? F7 P2 F7' F11 -152(3) . . . . ? F9 P2 F7' F11 91.5(6) . . . . ? F8 P2 F7' F11 -165.6(11) . . . . ? F8' P2 F11 F7' -41(2) . . . . ? F10 P2 F11 F7' -167.6(10) . . . . ? F12 P2 F11 F7' 95.3(10) . . . . ? F7 P2 F11 F7' 16.7(15) . . . . ? F9 P2 F11 F7' -84.0(10) . . . . ? F8 P2 F11 F7' 149(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O H1 F3 0.85(5) 2.07(5) 2.884(11) 159(8) 3_656 O H1 F5 0.85(5) 2.20(7) 2.924(10) 143(8) 3_656 O H2 F1 0.92(5) 1.75(5) 2.652(9) 169(8) 4_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.233 _refine_diff_density_min -1.249 _refine_diff_density_rms 0.136 data_dippp _database_code_depnum_ccdc_archive 'CCDC 251480' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(2,2'-Bipyridine)(4,5-diphenylimidazole)(2,2':6',2''-terpyridine)- ruthenium(II)]bis(hexafluorophosphate).methanol ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C10 H8 N2)(C15 H12 N2)(C15 H11 N3)Ru](P F6)2.(CH3OH)' _chemical_formula_sum 'C41 H35 F12 N7 O P2 Ru' _chemical_formula_weight 1032.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinc _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.9571(12) _cell_length_b 13.7320(9) _cell_length_c 17.7831(11) _cell_angle_alpha 90.00 _cell_angle_beta 115.7650(10) _cell_angle_gamma 90.00 _cell_volume 4169.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour 'dark-red to black' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8838 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart AXS CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30258 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.06 _reflns_number_total 7394 _reflns_number_gt 5219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms on carbon and nitrogen were calculated using appropriate riding models (AFIX 43, U(H) = 1.2 Ueq(C/N). The hydrogen atoms of the methanol molecule were calculated with the riding models AFIX 137 (CH3) and AFIX 147 (OH, d(O-H) = 0.83 A) and isotropic temperature factors of U(H) = 1.5 Ueq(C/O). The position of the O-bonded H of the methanol molecule was refined with respect to a staggered conformation and an N-H???O and possible O-H???F hydrogen bridge. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0042P)^2^+12.0422P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7394 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.25442(2) 0.09619(3) -0.14413(2) 0.02781(10) Uani 1 1 d . . . N1 N 0.13978(19) 0.1091(3) -0.2340(2) 0.0315(8) Uani 1 1 d . . . N2 N 0.1996(2) 0.0279(2) -0.0885(2) 0.0288(8) Uani 1 1 d . . . N3 N 0.3479(2) 0.0632(3) -0.0301(2) 0.0305(8) Uani 1 1 d . . . N4 N 0.2731(2) -0.0325(3) -0.1936(2) 0.0342(9) Uani 1 1 d . . . N5 N 0.3079(2) 0.1466(3) -0.2183(2) 0.0332(9) Uani 1 1 d . . . N6 N 0.2554(2) 0.2333(2) -0.0885(2) 0.0286(8) Uani 1 1 d . . . N7 N 0.3108(2) 0.3712(3) -0.0281(2) 0.0330(9) Uani 1 1 d . . . H7A H 0.3457 0.4168 -0.0072 0.040 Uiso 1 1 calc R . . C1 C 0.1113(3) 0.1614(4) -0.3050(3) 0.0400(12) Uani 1 1 d . . . H1A H 0.1461 0.1989 -0.3179 0.048 Uiso 1 1 calc R . . C2 C 0.0327(3) 0.1617(4) -0.3596(3) 0.0530(14) Uani 1 1 d . . . H2A H 0.0146 0.1983 -0.4091 0.064 Uiso 1 1 calc R . . C3 C -0.0186(3) 0.1084(4) -0.3409(3) 0.0557(15) Uani 1 1 d . . . H3A H -0.0722 0.1076 -0.3778 0.067 Uiso 1 1 calc R . . C4 C 0.0089(3) 0.0559(4) -0.2676(3) 0.0425(12) Uani 1 1 d . . . H4A H -0.0259 0.0195 -0.2539 0.051 Uiso 1 1 calc R . . C5 C 0.0883(2) 0.0573(3) -0.2142(3) 0.0337(10) Uani 1 1 d . . . C6 C 0.1224(2) 0.0071(3) -0.1339(3) 0.0321(10) Uani 1 1 d . . . C7 C 0.0853(3) -0.0558(4) -0.1015(3) 0.0433(12) Uani 1 1 d . . . H7B H 0.0319 -0.0709 -0.1319 0.052 Uiso 1 1 calc R . . C8 C 0.1285(3) -0.0957(4) -0.0235(3) 0.0481(13) Uani 1 1 d . . . H8A H 0.1042 -0.1388 -0.0009 0.058 Uiso 1 1 calc R . . C9 C 0.2066(3) -0.0734(3) 0.0217(3) 0.0412(12) Uani 1 1 d . . . H9A H 0.2355 -0.1010 0.0748 0.049 Uiso 1 1 calc R . . C10 C 0.2420(3) -0.0101(3) -0.0117(3) 0.0337(10) Uani 1 1 d . . . C11 C 0.3247(3) 0.0201(3) 0.0250(3) 0.0298(10) Uani 1 1 d . . . C12 C 0.3761(3) 0.0081(3) 0.1079(3) 0.0412(12) Uani 1 1 d . . . H12A H 0.3589 -0.0205 0.1450 0.049 Uiso 1 1 calc R . . C13 C 0.4525(3) 0.0383(4) 0.1361(3) 0.0501(14) Uani 1 1 d . . . H13A H 0.4877 0.0316 0.1927 0.060 Uiso 1 1 calc R . . C14 C 0.4769(3) 0.0784(4) 0.0802(3) 0.0472(13) Uani 1 1 d . . . H14A H 0.5291 0.0985 0.0979 0.057 Uiso 1 1 calc R . . C15 C 0.4232(2) 0.0886(3) -0.0023(3) 0.0370(11) Uani 1 1 d . . . H15A H 0.4403 0.1145 -0.0405 0.044 Uiso 1 1 calc R . . C16 C 0.2556(3) -0.1224(3) -0.1768(3) 0.0438(12) Uani 1 1 d . . . H16A H 0.2277 -0.1284 -0.1444 0.053 Uiso 1 1 calc R . . C17 C 0.2765(3) -0.2051(4) -0.2045(3) 0.0542(14) Uani 1 1 d . . . H17A H 0.2622 -0.2665 -0.1922 0.065 Uiso 1 1 calc R . . C18 C 0.3184(3) -0.1980(4) -0.2505(3) 0.0542(15) Uani 1 1 d . . . H18A H 0.3338 -0.2542 -0.2696 0.065 Uiso 1 1 calc R . . C19 C 0.3374(3) -0.1074(4) -0.2683(3) 0.0455(13) Uani 1 1 d . . . H19A H 0.3661 -0.1012 -0.2998 0.055 Uiso 1 1 calc R . . C20 C 0.3144(2) -0.0246(4) -0.2398(3) 0.0349(11) Uani 1 1 d . . . C21 C 0.3304(2) 0.0749(4) -0.2565(3) 0.0364(11) Uani 1 1 d . . . C22 C 0.3637(3) 0.0983(4) -0.3100(3) 0.0440(12) Uani 1 1 d . . . H22A H 0.3803 0.0484 -0.3348 0.053 Uiso 1 1 calc R . . C23 C 0.3726(3) 0.1938(5) -0.3269(3) 0.0551(15) Uani 1 1 d . . . H23A H 0.3959 0.2099 -0.3623 0.066 Uiso 1 1 calc R . . C24 C 0.3467(3) 0.2656(4) -0.2908(3) 0.0519(14) Uani 1 1 d . . . H24A H 0.3511 0.3316 -0.3021 0.062 Uiso 1 1 calc R . . C25 C 0.3141(3) 0.2391(4) -0.2378(3) 0.0409(12) Uani 1 1 d . . . H25A H 0.2955 0.2883 -0.2145 0.049 Uiso 1 1 calc R . . C26 C 0.3202(2) 0.2879(3) -0.0608(3) 0.0327(10) Uani 1 1 d . . . H26A H 0.3666 0.2698 -0.0641 0.039 Uiso 1 1 calc R . . C27 C 0.2362(2) 0.3730(3) -0.0327(3) 0.0324(10) Uani 1 1 d . . . C28 C 0.2026(2) 0.2868(3) -0.0701(3) 0.0296(10) Uani 1 1 d . . . C29 C 0.2075(2) 0.4565(3) -0.0024(3) 0.0335(10) Uani 1 1 d . . . C30 C 0.1528(3) 0.4455(4) 0.0298(3) 0.0407(12) Uani 1 1 d . . . H30A H 0.1329 0.3834 0.0319 0.049 Uiso 1 1 calc R . . C31 C 0.1275(3) 0.5259(4) 0.0586(3) 0.0482(13) Uani 1 1 d . . . H31A H 0.0901 0.5178 0.0797 0.058 Uiso 1 1 calc R . . C32 C 0.1561(3) 0.6164(4) 0.0567(3) 0.0479(13) Uani 1 1 d . . . H32A H 0.1390 0.6703 0.0769 0.057 Uiso 1 1 calc R . . C33 C 0.2105(3) 0.6291(4) 0.0248(3) 0.0460(13) Uani 1 1 d . . . H33A H 0.2305 0.6914 0.0237 0.055 Uiso 1 1 calc R . . C34 C 0.2351(3) 0.5499(3) -0.0054(3) 0.0368(11) Uani 1 1 d . . . H34A H 0.2710 0.5591 -0.0282 0.044 Uiso 1 1 calc R . . C35 C 0.1216(3) 0.2557(3) -0.0901(3) 0.0320(10) Uani 1 1 d . . . C36 C 0.1060(3) 0.1934(3) -0.0380(3) 0.0442(12) Uani 1 1 d . . . H36A H 0.1476 0.1672 0.0094 0.053 Uiso 1 1 calc R . . C37 C 0.0296(3) 0.1696(4) -0.0554(4) 0.0588(17) Uani 1 1 d . . . H37A H 0.0196 0.1265 -0.0202 0.071 Uiso 1 1 calc R . . C38 C -0.0316(3) 0.2086(4) -0.1238(5) 0.0667(19) Uani 1 1 d . . . H38A H -0.0834 0.1919 -0.1353 0.080 Uiso 1 1 calc R . . C39 C -0.0172(3) 0.2718(5) -0.1751(4) 0.0623(17) Uani 1 1 d . . . H39A H -0.0591 0.2991 -0.2215 0.075 Uiso 1 1 calc R . . C40 C 0.0594(3) 0.2954(4) -0.1586(3) 0.0447(12) Uani 1 1 d . . . H40A H 0.0691 0.3386 -0.1940 0.054 Uiso 1 1 calc R . . C41 C 0.5272(4) 0.4349(6) 0.1181(4) 0.100(3) Uani 1 1 d . . . H41A H 0.5632 0.4582 0.0967 0.150 Uiso 1 1 calc R . . H41B H 0.5260 0.3643 0.1168 0.150 Uiso 1 1 calc R . . H41C H 0.5444 0.4571 0.1752 0.150 Uiso 1 1 calc R . . O O 0.4513(2) 0.4713(3) 0.0682(3) 0.0768(13) Uani 1 1 d . . . H0 H 0.4540 0.5306 0.0608 0.115 Uiso 1 1 calc R . . P1 P 0.80467(8) 0.51027(11) 0.27373(9) 0.0482(4) Uani 1 1 d . . . P2 P 0.43767(9) 0.74729(11) 0.07605(11) 0.0572(4) Uani 1 1 d . . . F1 F 0.8271(3) 0.6106(3) 0.2463(3) 0.1057(14) Uani 1 1 d . . . F2 F 0.7206(2) 0.5220(4) 0.2009(2) 0.1078(15) Uani 1 1 d . . . F3 F 0.8325(2) 0.4525(3) 0.2141(2) 0.0871(12) Uani 1 1 d . . . F4 F 0.8895(2) 0.5016(3) 0.3469(2) 0.0946(13) Uani 1 1 d . . . F5 F 0.7781(2) 0.5670(2) 0.3350(2) 0.0758(10) Uani 1 1 d . . . F6 F 0.7823(2) 0.4097(2) 0.3009(2) 0.0812(11) Uani 1 1 d . . . F7 F 0.3811(2) 0.6705(3) 0.0106(3) 0.1005(14) Uani 1 1 d . . . F8 F 0.4149(2) 0.8266(3) 0.0050(2) 0.0869(11) Uani 1 1 d . . . F9 F 0.5074(2) 0.7080(3) 0.0587(3) 0.0928(13) Uani 1 1 d . . . F10 F 0.49531(19) 0.8240(2) 0.1390(2) 0.0792(11) Uani 1 1 d . . . F11 F 0.3679(2) 0.7843(3) 0.0953(3) 0.0908(12) Uani 1 1 d . . . F12 F 0.4592(3) 0.6691(3) 0.1485(3) 0.1041(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.02662(18) 0.03010(19) 0.02877(19) -0.00060(17) 0.01395(15) 0.00212(16) N1 0.0278(19) 0.034(2) 0.032(2) -0.0036(18) 0.0127(16) 0.0051(17) N2 0.029(2) 0.029(2) 0.031(2) -0.0044(16) 0.0162(17) 0.0030(16) N3 0.030(2) 0.033(2) 0.030(2) -0.0029(16) 0.0140(17) 0.0043(16) N4 0.035(2) 0.039(2) 0.026(2) -0.0032(17) 0.0108(17) 0.0053(17) N5 0.027(2) 0.040(2) 0.031(2) 0.0023(18) 0.0115(17) 0.0033(17) N6 0.028(2) 0.030(2) 0.031(2) 0.0008(16) 0.0163(17) 0.0024(16) N7 0.030(2) 0.030(2) 0.039(2) 0.0005(17) 0.0145(18) -0.0039(16) C1 0.039(3) 0.050(3) 0.031(3) 0.000(2) 0.014(2) 0.005(2) C2 0.046(3) 0.071(4) 0.035(3) 0.004(3) 0.011(3) 0.013(3) C3 0.036(3) 0.076(4) 0.043(3) -0.011(3) 0.006(2) 0.007(3) C4 0.032(3) 0.047(3) 0.045(3) -0.009(2) 0.014(2) -0.001(2) C5 0.028(2) 0.035(3) 0.038(3) -0.008(2) 0.014(2) -0.001(2) C6 0.030(2) 0.031(2) 0.040(3) -0.005(2) 0.020(2) 0.0006(19) C7 0.037(3) 0.046(3) 0.054(3) -0.009(3) 0.027(3) -0.010(2) C8 0.054(3) 0.043(3) 0.065(4) 0.005(3) 0.043(3) -0.004(3) C9 0.051(3) 0.040(3) 0.043(3) 0.003(2) 0.030(3) 0.004(2) C10 0.037(3) 0.033(3) 0.035(3) -0.004(2) 0.019(2) 0.002(2) C11 0.035(2) 0.029(2) 0.028(2) 0.0019(19) 0.016(2) 0.0068(19) C12 0.049(3) 0.042(3) 0.035(3) 0.002(2) 0.021(2) 0.008(2) C13 0.045(3) 0.062(4) 0.033(3) 0.000(3) 0.006(2) 0.008(3) C14 0.033(3) 0.052(3) 0.046(3) -0.002(3) 0.007(2) 0.006(2) C15 0.031(2) 0.039(3) 0.043(3) 0.002(2) 0.018(2) 0.005(2) C16 0.053(3) 0.040(3) 0.039(3) -0.005(2) 0.021(3) 0.003(2) C17 0.066(4) 0.041(3) 0.050(3) -0.013(3) 0.020(3) 0.002(3) C18 0.049(3) 0.051(4) 0.053(3) -0.020(3) 0.013(3) 0.009(3) C19 0.035(3) 0.061(4) 0.037(3) -0.019(3) 0.012(2) 0.008(3) C20 0.025(2) 0.050(3) 0.026(2) -0.007(2) 0.007(2) 0.006(2) C21 0.024(2) 0.057(3) 0.025(2) -0.007(2) 0.0078(19) 0.000(2) C22 0.036(3) 0.068(4) 0.035(3) -0.006(3) 0.021(2) 0.001(3) C23 0.046(3) 0.090(5) 0.039(3) 0.005(3) 0.028(3) -0.003(3) C24 0.048(3) 0.065(4) 0.047(3) 0.013(3) 0.025(3) -0.004(3) C25 0.046(3) 0.043(3) 0.041(3) 0.011(2) 0.026(2) 0.007(2) C26 0.028(2) 0.033(3) 0.042(3) 0.002(2) 0.020(2) 0.004(2) C27 0.027(2) 0.036(3) 0.035(3) -0.005(2) 0.013(2) -0.0021(19) C28 0.029(2) 0.029(2) 0.031(2) 0.001(2) 0.012(2) 0.0015(19) C29 0.029(2) 0.036(3) 0.031(3) 0.000(2) 0.008(2) 0.001(2) C30 0.047(3) 0.036(3) 0.048(3) -0.006(2) 0.029(3) -0.002(2) C31 0.050(3) 0.051(3) 0.052(3) -0.004(3) 0.030(3) 0.006(3) C32 0.042(3) 0.048(3) 0.044(3) -0.015(2) 0.010(2) 0.008(2) C33 0.040(3) 0.036(3) 0.051(3) -0.009(2) 0.009(3) -0.002(2) C34 0.027(2) 0.037(3) 0.042(3) -0.005(2) 0.011(2) -0.002(2) C35 0.032(3) 0.028(2) 0.044(3) -0.009(2) 0.023(2) 0.0017(19) C36 0.050(3) 0.040(3) 0.059(3) -0.005(3) 0.038(3) -0.002(2) C37 0.066(4) 0.039(3) 0.104(5) -0.012(3) 0.068(4) -0.009(3) C38 0.045(4) 0.057(4) 0.115(6) -0.035(4) 0.050(4) -0.017(3) C39 0.033(3) 0.073(4) 0.077(4) -0.017(3) 0.021(3) 0.000(3) C40 0.037(3) 0.043(3) 0.053(3) -0.003(3) 0.019(3) 0.001(2) C41 0.058(4) 0.156(8) 0.088(5) -0.019(5) 0.034(4) -0.008(5) O 0.059(3) 0.063(3) 0.103(4) -0.012(3) 0.029(3) -0.021(2) P1 0.0450(8) 0.0561(9) 0.0488(8) 0.0127(7) 0.0254(7) 0.0083(7) P2 0.0440(8) 0.0515(9) 0.0829(12) -0.0049(8) 0.0342(8) -0.0095(7) F1 0.128(4) 0.087(3) 0.137(4) 0.040(3) 0.091(3) 0.002(3) F2 0.058(2) 0.165(4) 0.076(3) 0.017(3) 0.006(2) 0.022(3) F3 0.092(3) 0.113(3) 0.075(2) -0.003(2) 0.053(2) 0.016(2) F4 0.063(2) 0.097(3) 0.090(3) -0.011(2) 0.002(2) 0.018(2) F5 0.103(3) 0.063(2) 0.083(2) 0.0106(19) 0.060(2) 0.021(2) F6 0.129(3) 0.058(2) 0.079(2) -0.0119(19) 0.065(2) -0.022(2) F7 0.065(2) 0.088(3) 0.147(4) -0.047(3) 0.045(3) -0.032(2) F8 0.075(2) 0.102(3) 0.074(3) 0.015(2) 0.022(2) -0.006(2) F9 0.064(2) 0.090(3) 0.149(4) -0.030(3) 0.070(3) -0.012(2) F10 0.064(2) 0.063(2) 0.085(3) -0.0098(19) 0.0082(19) -0.0083(18) F11 0.074(2) 0.080(3) 0.147(4) -0.006(2) 0.074(3) -0.002(2) F12 0.121(3) 0.074(3) 0.143(4) 0.031(3) 0.082(3) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 1.957(3) . ? Ru N1 2.071(3) . ? Ru N4 2.072(4) . ? Ru N3 2.082(3) . ? Ru N5 2.100(4) . ? Ru N6 2.124(3) . ? N1 C1 1.344(5) . ? N1 C5 1.372(5) . ? N2 C10 1.353(5) . ? N2 C6 1.360(5) . ? N3 C15 1.338(5) . ? N3 C11 1.371(5) . ? N4 C16 1.345(6) . ? N4 C20 1.362(5) . ? N5 C25 1.334(6) . ? N5 C21 1.365(6) . ? N6 C26 1.338(5) . ? N6 C28 1.390(5) . ? N7 C26 1.330(5) . ? N7 C27 1.378(5) . ? N7 H7A 0.8700 . ? C1 C2 1.380(6) . ? C1 H1A 0.9400 . ? C2 C3 1.369(7) . ? C2 H2A 0.9400 . ? C3 C4 1.378(7) . ? C3 H3A 0.9400 . ? C4 C5 1.387(6) . ? C4 H4A 0.9400 . ? C5 C6 1.459(6) . ? C6 C7 1.387(6) . ? C7 C8 1.381(7) . ? C7 H7B 0.9400 . ? C8 C9 1.378(7) . ? C8 H8A 0.9400 . ? C9 C10 1.379(6) . ? C9 H9A 0.9400 . ? C10 C11 1.473(6) . ? C11 C12 1.378(6) . ? C12 C13 1.375(7) . ? C12 H12A 0.9400 . ? C13 C14 1.380(7) . ? C13 H13A 0.9400 . ? C14 C15 1.381(6) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C16 C17 1.364(7) . ? C16 H16A 0.9400 . ? C17 C18 1.370(7) . ? C17 H17A 0.9400 . ? C18 C19 1.370(7) . ? C18 H18A 0.9400 . ? C19 C20 1.389(6) . ? C19 H19A 0.9400 . ? C20 C21 1.458(7) . ? C21 C22 1.390(6) . ? C22 C23 1.372(7) . ? C22 H22A 0.9400 . ? C23 C24 1.377(7) . ? C23 H23A 0.9400 . ? C24 C25 1.382(6) . ? C24 H24A 0.9400 . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C27 C28 1.372(6) . ? C27 C29 1.470(6) . ? C28 C35 1.480(6) . ? C29 C34 1.395(6) . ? C29 C30 1.395(6) . ? C30 C31 1.387(6) . ? C30 H30A 0.9400 . ? C31 C32 1.363(7) . ? C31 H31A 0.9400 . ? C32 C33 1.386(7) . ? C32 H32A 0.9400 . ? C33 C34 1.380(6) . ? C33 H33A 0.9400 . ? C34 H34A 0.9400 . ? C35 C36 1.383(6) . ? C35 C40 1.387(6) . ? C36 C37 1.382(7) . ? C36 H36A 0.9400 . ? C37 C38 1.373(8) . ? C37 H37A 0.9400 . ? C38 C39 1.371(8) . ? C38 H38A 0.9400 . ? C39 C40 1.388(7) . ? C39 H39A 0.9400 . ? C40 H40A 0.9400 . ? C41 O 1.413(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? O H0 0.8300 . ? P1 F2 1.565(4) . ? P1 F4 1.573(4) . ? P1 F1 1.580(4) . ? P1 F6 1.582(3) . ? P1 F3 1.587(4) . ? P1 F5 1.590(3) . ? P2 F9 1.577(3) . ? P2 F10 1.579(3) . ? P2 F8 1.579(4) . ? P2 F11 1.587(4) . ? P2 F12 1.588(4) . ? P2 F7 1.591(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru N1 79.73(14) . . ? N2 Ru N4 91.85(14) . . ? N1 Ru N4 93.51(14) . . ? N2 Ru N3 79.52(14) . . ? N1 Ru N3 159.07(14) . . ? N4 Ru N3 89.87(13) . . ? N2 Ru N5 169.31(14) . . ? N1 Ru N5 96.77(14) . . ? N4 Ru N5 78.22(15) . . ? N3 Ru N5 104.14(13) . . ? N2 Ru N6 95.09(13) . . ? N1 Ru N6 94.42(13) . . ? N4 Ru N6 170.28(14) . . ? N3 Ru N6 84.72(13) . . ? N5 Ru N6 95.25(14) . . ? C1 N1 C5 118.6(4) . . ? C1 N1 Ru 128.9(3) . . ? C5 N1 Ru 112.5(3) . . ? C10 N2 C6 122.1(4) . . ? C10 N2 Ru 118.9(3) . . ? C6 N2 Ru 118.2(3) . . ? C15 N3 C11 118.0(4) . . ? C15 N3 Ru 128.6(3) . . ? C11 N3 Ru 112.8(3) . . ? C16 N4 C20 117.9(4) . . ? C16 N4 Ru 125.7(3) . . ? C20 N4 Ru 116.0(3) . . ? C25 N5 C21 118.4(4) . . ? C25 N5 Ru 126.8(3) . . ? C21 N5 Ru 114.5(3) . . ? C26 N6 C28 105.0(3) . . ? C26 N6 Ru 119.3(3) . . ? C28 N6 Ru 135.8(3) . . ? C26 N7 C27 108.6(4) . . ? C26 N7 H7A 125.7 . . ? C27 N7 H7A 125.7 . . ? N1 C1 C2 122.1(5) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C3 C2 C1 119.4(5) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 119.4(5) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? N1 C5 C4 120.9(4) . . ? N1 C5 C6 115.7(4) . . ? C4 C5 C6 123.4(4) . . ? N2 C6 C7 119.6(4) . . ? N2 C6 C5 112.7(4) . . ? C7 C6 C5 127.7(4) . . ? C8 C7 C6 118.6(5) . . ? C8 C7 H7B 120.7 . . ? C6 C7 H7B 120.7 . . ? C9 C8 C7 121.0(5) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? N2 C10 C9 119.5(4) . . ? N2 C10 C11 112.9(4) . . ? C9 C10 C11 127.6(4) . . ? N3 C11 C12 121.3(4) . . ? N3 C11 C10 114.6(4) . . ? C12 C11 C10 124.1(4) . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 119.2(5) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C13 C14 C15 118.8(5) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? N3 C15 C14 122.8(4) . . ? N3 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? N4 C16 C17 123.1(5) . . ? N4 C16 H16A 118.5 . . ? C17 C16 H16A 118.5 . . ? C16 C17 C18 119.4(5) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C19 C18 C17 118.8(5) . . ? C19 C18 H18A 120.6 . . ? C17 C18 H18A 120.6 . . ? C18 C19 C20 120.2(5) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? N4 C20 C19 120.6(5) . . ? N4 C20 C21 114.9(4) . . ? C19 C20 C21 124.5(4) . . ? N5 C21 C22 120.4(5) . . ? N5 C21 C20 116.0(4) . . ? C22 C21 C20 123.5(4) . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 118.7(5) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C23 C24 C25 118.9(5) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N5 C25 C24 123.0(5) . . ? N5 C25 H25A 118.5 . . ? C24 C25 H25A 118.5 . . ? N7 C26 N6 111.4(4) . . ? N7 C26 H26A 124.3 . . ? N6 C26 H26A 124.3 . . ? C28 C27 N7 105.2(4) . . ? C28 C27 C29 133.1(4) . . ? N7 C27 C29 121.7(4) . . ? C27 C28 N6 109.8(4) . . ? C27 C28 C35 125.5(4) . . ? N6 C28 C35 124.7(4) . . ? C34 C29 C30 118.3(4) . . ? C34 C29 C27 120.0(4) . . ? C30 C29 C27 121.8(4) . . ? C31 C30 C29 120.2(5) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C32 C31 C30 120.7(5) . . ? C32 C31 H31A 119.6 . . ? C30 C31 H31A 119.6 . . ? C31 C32 C33 120.0(5) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 119.8(5) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C33 C34 C29 120.9(4) . . ? C33 C34 H34A 119.5 . . ? C29 C34 H34A 119.5 . . ? C36 C35 C40 119.0(4) . . ? C36 C35 C28 121.2(4) . . ? C40 C35 C28 119.6(4) . . ? C37 C36 C35 120.2(5) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C38 C37 C36 120.4(5) . . ? C38 C37 H37A 119.8 . . ? C36 C37 H37A 119.8 . . ? C39 C38 C37 120.0(5) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C40 120.0(6) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C35 C40 C39 120.3(5) . . ? C35 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? O C41 H41A 109.5 . . ? O C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 O H0 109.5 . . ? F2 P1 F4 178.4(3) . . ? F2 P1 F1 88.2(3) . . ? F4 P1 F1 90.3(2) . . ? F2 P1 F6 91.8(2) . . ? F4 P1 F6 89.7(2) . . ? F1 P1 F6 179.8(2) . . ? F2 P1 F3 90.8(2) . . ? F4 P1 F3 89.9(2) . . ? F1 P1 F3 91.0(2) . . ? F6 P1 F3 88.8(2) . . ? F2 P1 F5 90.2(2) . . ? F4 P1 F5 89.1(2) . . ? F1 P1 F5 89.6(2) . . ? F6 P1 F5 90.64(18) . . ? F3 P1 F5 178.9(2) . . ? F9 P2 F10 89.2(2) . . ? F9 P2 F8 92.3(2) . . ? F10 P2 F8 88.4(2) . . ? F9 P2 F11 178.4(3) . . ? F10 P2 F11 91.0(2) . . ? F8 P2 F11 89.3(2) . . ? F9 P2 F12 89.2(2) . . ? F10 P2 F12 91.2(2) . . ? F8 P2 F12 178.4(2) . . ? F11 P2 F12 89.2(2) . . ? F9 P2 F7 89.2(2) . . ? F10 P2 F7 178.0(2) . . ? F8 P2 F7 90.5(2) . . ? F11 P2 F7 90.6(2) . . ? F12 P2 F7 89.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru N1 C1 172.0(4) . . . . ? N4 Ru N1 C1 -96.7(4) . . . . ? N3 Ru N1 C1 164.4(4) . . . . ? N5 Ru N1 C1 -18.2(4) . . . . ? N6 Ru N1 C1 77.7(4) . . . . ? N2 Ru N1 C5 -6.5(3) . . . . ? N4 Ru N1 C5 84.8(3) . . . . ? N3 Ru N1 C5 -14.1(6) . . . . ? N5 Ru N1 C5 163.3(3) . . . . ? N6 Ru N1 C5 -100.9(3) . . . . ? N1 Ru N2 C10 179.9(3) . . . . ? N4 Ru N2 C10 86.6(3) . . . . ? N3 Ru N2 C10 -2.9(3) . . . . ? N5 Ru N2 C10 108.2(8) . . . . ? N6 Ru N2 C10 -86.6(3) . . . . ? N1 Ru N2 C6 10.2(3) . . . . ? N4 Ru N2 C6 -83.0(3) . . . . ? N3 Ru N2 C6 -172.6(3) . . . . ? N5 Ru N2 C6 -61.5(9) . . . . ? N6 Ru N2 C6 103.8(3) . . . . ? N2 Ru N3 C15 -176.0(4) . . . . ? N1 Ru N3 C15 -168.4(4) . . . . ? N4 Ru N3 C15 92.1(4) . . . . ? N5 Ru N3 C15 14.3(4) . . . . ? N6 Ru N3 C15 -79.8(4) . . . . ? N2 Ru N3 C11 -4.6(3) . . . . ? N1 Ru N3 C11 3.1(6) . . . . ? N4 Ru N3 C11 -96.5(3) . . . . ? N5 Ru N3 C11 -174.3(3) . . . . ? N6 Ru N3 C11 91.6(3) . . . . ? N2 Ru N4 C16 -5.7(4) . . . . ? N1 Ru N4 C16 -85.5(4) . . . . ? N3 Ru N4 C16 73.8(4) . . . . ? N5 Ru N4 C16 178.3(4) . . . . ? N6 Ru N4 C16 129.8(8) . . . . ? N2 Ru N4 C20 -178.2(3) . . . . ? N1 Ru N4 C20 101.9(3) . . . . ? N3 Ru N4 C20 -98.7(3) . . . . ? N5 Ru N4 C20 5.7(3) . . . . ? N6 Ru N4 C20 -42.7(9) . . . . ? N2 Ru N5 C25 147.7(7) . . . . ? N1 Ru N5 C25 77.6(4) . . . . ? N4 Ru N5 C25 169.8(4) . . . . ? N3 Ru N5 C25 -103.4(4) . . . . ? N6 Ru N5 C25 -17.5(4) . . . . ? N2 Ru N5 C21 -24.9(9) . . . . ? N1 Ru N5 C21 -95.0(3) . . . . ? N4 Ru N5 C21 -2.8(3) . . . . ? N3 Ru N5 C21 84.0(3) . . . . ? N6 Ru N5 C21 169.9(3) . . . . ? N2 Ru N6 C26 137.8(3) . . . . ? N1 Ru N6 C26 -142.1(3) . . . . ? N4 Ru N6 C26 2.5(10) . . . . ? N3 Ru N6 C26 58.9(3) . . . . ? N5 Ru N6 C26 -44.9(3) . . . . ? N2 Ru N6 C28 -41.1(4) . . . . ? N1 Ru N6 C28 39.0(4) . . . . ? N4 Ru N6 C28 -176.4(7) . . . . ? N3 Ru N6 C28 -120.0(4) . . . . ? N5 Ru N6 C28 136.2(4) . . . . ? C5 N1 C1 C2 -2.3(7) . . . . ? Ru N1 C1 C2 179.2(4) . . . . ? N1 C1 C2 C3 0.9(8) . . . . ? C1 C2 C3 C4 0.6(8) . . . . ? C2 C3 C4 C5 -0.6(8) . . . . ? C1 N1 C5 C4 2.3(6) . . . . ? Ru N1 C5 C4 -179.0(3) . . . . ? C1 N1 C5 C6 -176.3(4) . . . . ? Ru N1 C5 C6 2.4(5) . . . . ? C3 C4 C5 N1 -0.9(7) . . . . ? C3 C4 C5 C6 177.6(4) . . . . ? C10 N2 C6 C7 -0.8(6) . . . . ? Ru N2 C6 C7 168.6(3) . . . . ? C10 N2 C6 C5 179.1(4) . . . . ? Ru N2 C6 C5 -11.6(5) . . . . ? N1 C5 C6 N2 5.5(5) . . . . ? C4 C5 C6 N2 -173.0(4) . . . . ? N1 C5 C6 C7 -174.7(4) . . . . ? C4 C5 C6 C7 6.8(7) . . . . ? N2 C6 C7 C8 -0.1(7) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? C6 C7 C8 C9 0.4(7) . . . . ? C7 C8 C9 C10 0.0(7) . . . . ? C6 N2 C10 C9 1.2(6) . . . . ? Ru N2 C10 C9 -168.1(3) . . . . ? C6 N2 C10 C11 178.5(4) . . . . ? Ru N2 C10 C11 9.3(5) . . . . ? C8 C9 C10 N2 -0.8(7) . . . . ? C8 C9 C10 C11 -177.7(4) . . . . ? C15 N3 C11 C12 3.6(6) . . . . ? Ru N3 C11 C12 -168.7(3) . . . . ? C15 N3 C11 C10 -177.0(4) . . . . ? Ru N3 C11 C10 10.6(4) . . . . ? N2 C10 C11 N3 -13.0(5) . . . . ? C9 C10 C11 N3 164.1(4) . . . . ? N2 C10 C11 C12 166.4(4) . . . . ? C9 C10 C11 C12 -16.6(7) . . . . ? N3 C11 C12 C13 -1.1(7) . . . . ? C10 C11 C12 C13 179.6(4) . . . . ? C11 C12 C13 C14 -1.3(7) . . . . ? C12 C13 C14 C15 1.1(8) . . . . ? C11 N3 C15 C14 -3.9(7) . . . . ? Ru N3 C15 C14 167.1(4) . . . . ? C13 C14 C15 N3 1.5(7) . . . . ? C20 N4 C16 C17 -0.7(7) . . . . ? Ru N4 C16 C17 -173.1(4) . . . . ? N4 C16 C17 C18 1.2(8) . . . . ? C16 C17 C18 C19 -0.8(8) . . . . ? C17 C18 C19 C20 0.0(7) . . . . ? C16 N4 C20 C19 -0.1(6) . . . . ? Ru N4 C20 C19 173.0(3) . . . . ? C16 N4 C20 C21 179.3(4) . . . . ? Ru N4 C20 C21 -7.6(5) . . . . ? C18 C19 C20 N4 0.4(7) . . . . ? C18 C19 C20 C21 -178.9(5) . . . . ? C25 N5 C21 C22 4.2(6) . . . . ? Ru N5 C21 C22 177.5(3) . . . . ? C25 N5 C21 C20 -173.5(4) . . . . ? Ru N5 C21 C20 -0.2(5) . . . . ? N4 C20 C21 N5 5.1(6) . . . . ? C19 C20 C21 N5 -175.6(4) . . . . ? N4 C20 C21 C22 -172.5(4) . . . . ? C19 C20 C21 C22 6.8(7) . . . . ? N5 C21 C22 C23 -1.7(7) . . . . ? C20 C21 C22 C23 175.8(4) . . . . ? C21 C22 C23 C24 -1.0(8) . . . . ? C22 C23 C24 C25 1.2(8) . . . . ? C21 N5 C25 C24 -4.1(7) . . . . ? Ru N5 C25 C24 -176.5(4) . . . . ? C23 C24 C25 N5 1.4(8) . . . . ? C27 N7 C26 N6 0.7(5) . . . . ? C28 N6 C26 N7 -0.9(5) . . . . ? Ru N6 C26 N7 179.9(3) . . . . ? C26 N7 C27 C28 -0.2(5) . . . . ? C26 N7 C27 C29 -179.2(4) . . . . ? N7 C27 C28 N6 -0.4(5) . . . . ? C29 C27 C28 N6 178.5(4) . . . . ? N7 C27 C28 C35 -178.9(4) . . . . ? C29 C27 C28 C35 -0.1(8) . . . . ? C26 N6 C28 C27 0.8(5) . . . . ? Ru N6 C28 C27 179.8(3) . . . . ? C26 N6 C28 C35 179.4(4) . . . . ? Ru N6 C28 C35 -1.7(7) . . . . ? C28 C27 C29 C34 -148.1(5) . . . . ? N7 C27 C29 C34 30.6(6) . . . . ? C28 C27 C29 C30 31.9(8) . . . . ? N7 C27 C29 C30 -149.4(4) . . . . ? C34 C29 C30 C31 -0.6(7) . . . . ? C27 C29 C30 C31 179.4(4) . . . . ? C29 C30 C31 C32 -0.6(8) . . . . ? C30 C31 C32 C33 0.7(8) . . . . ? C31 C32 C33 C34 0.4(8) . . . . ? C32 C33 C34 C29 -1.6(7) . . . . ? C30 C29 C34 C33 1.7(7) . . . . ? C27 C29 C34 C33 -178.3(4) . . . . ? C27 C28 C35 C36 -98.1(6) . . . . ? N6 C28 C35 C36 83.6(6) . . . . ? C27 C28 C35 C40 76.7(6) . . . . ? N6 C28 C35 C40 -101.6(5) . . . . ? C40 C35 C36 C37 1.6(7) . . . . ? C28 C35 C36 C37 176.4(4) . . . . ? C35 C36 C37 C38 -1.0(8) . . . . ? C36 C37 C38 C39 -0.2(8) . . . . ? C37 C38 C39 C40 0.8(9) . . . . ? C36 C35 C40 C39 -1.0(7) . . . . ? C28 C35 C40 C39 -175.9(4) . . . . ? C38 C39 C40 C35 -0.2(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.935 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.091 data_yangbm _database_code_depnum_ccdc_archive 'CCDC 251481' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(2,2'-Bipyridine)(indazole)(2,2':6',2''-terpyridine)- ruthenium(II)]bis(hexafluorophosphate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C10 H8 N2)(C7 H6 N2)(C15 H11 N3)Ru](P F6)2' _chemical_formula_sum 'C32 H25 F12 N7 P2 Ru' _chemical_formula_weight 898.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 35.704(3) _cell_length_b 10.4729(8) _cell_length_c 18.4357(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6893.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8045 _exptl_absorpt_correction_T_max 0.8810 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart AXS CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22273 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 26.55 _reflns_number_total 6978 _reflns_number_gt 4990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms on carbon and nitrogen were calculated using appropriate riding models (AFIX 43, U(H) = 1.2 Ueq(C/N). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+7.6673P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6978 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.617051(8) 0.72349(2) 0.734662(17) 0.03044(10) Uani 1 1 d . . . N1 N 0.59663(9) 0.7404(3) 0.63011(17) 0.0344(7) Uani 1 1 d . . . N2 N 0.64222(8) 0.8818(2) 0.70418(17) 0.0333(7) Uani 1 1 d . . . N3 N 0.64667(9) 0.7664(3) 0.82790(17) 0.0358(7) Uani 1 1 d . . . N4 N 0.57125(9) 0.8132(3) 0.77884(17) 0.0353(7) Uani 1 1 d . . . N5 N 0.58561(9) 0.5684(3) 0.77021(16) 0.0340(7) Uani 1 1 d . . . N6 N 0.66142(8) 0.6119(2) 0.69723(17) 0.0338(7) Uani 1 1 d . . . C1 C 0.57456(11) 0.6593(4) 0.5937(2) 0.0407(9) Uani 1 1 d . . . H1A H 0.5677 0.5820 0.6160 0.049 Uiso 1 1 calc R . . C2 C 0.56150(14) 0.6845(4) 0.5250(3) 0.0547(11) Uani 1 1 d . . . H2A H 0.5462 0.6251 0.5008 0.066 Uiso 1 1 calc R . . C3 C 0.57108(14) 0.7978(4) 0.4925(3) 0.0600(13) Uani 1 1 d . . . H3A H 0.5616 0.8184 0.4463 0.072 Uiso 1 1 calc R . . C4 C 0.59482(13) 0.8817(4) 0.5280(2) 0.0506(11) Uani 1 1 d . . . H4A H 0.6021 0.9585 0.5058 0.061 Uiso 1 1 calc R . . C5 C 0.60764(11) 0.8512(3) 0.5963(2) 0.0372(9) Uani 1 1 d . . . C6 C 0.63393(11) 0.9305(3) 0.6382(2) 0.0371(9) Uani 1 1 d . . . C7 C 0.64968(12) 1.0460(4) 0.6176(2) 0.0471(10) Uani 1 1 d . . . H7A H 0.6441 1.0816 0.5721 0.057 Uiso 1 1 calc R . . C8 C 0.67355(13) 1.1081(4) 0.6645(3) 0.0544(12) Uani 1 1 d . . . H8A H 0.6846 1.1859 0.6506 0.065 Uiso 1 1 calc R . . C9 C 0.68146(12) 1.0568(4) 0.7319(2) 0.0483(10) Uani 1 1 d . . . H9A H 0.6975 1.0997 0.7642 0.058 Uiso 1 1 calc R . . C10 C 0.66534(11) 0.9413(3) 0.7511(2) 0.0375(9) Uani 1 1 d . . . C11 C 0.66905(11) 0.8732(3) 0.8208(2) 0.0380(9) Uani 1 1 d . . . C12 C 0.69244(12) 0.9108(4) 0.8764(2) 0.0503(11) Uani 1 1 d . . . H12A H 0.7080 0.9824 0.8703 0.060 Uiso 1 1 calc R . . C13 C 0.69304(14) 0.8438(5) 0.9407(3) 0.0577(12) Uani 1 1 d . . . H13A H 0.7092 0.8685 0.9784 0.069 Uiso 1 1 calc R . . C14 C 0.66962(14) 0.7404(4) 0.9492(2) 0.0538(11) Uani 1 1 d . . . H14A H 0.6691 0.6948 0.9932 0.065 Uiso 1 1 calc R . . C15 C 0.64698(12) 0.7050(4) 0.8920(2) 0.0423(9) Uani 1 1 d . . . H15A H 0.6310 0.6346 0.8981 0.051 Uiso 1 1 calc R . . C16 C 0.56477(12) 0.9405(3) 0.7801(2) 0.0486(11) Uani 1 1 d . . . H16A H 0.5811 0.9946 0.7544 0.058 Uiso 1 1 calc R . . C17 C 0.53538(13) 0.9937(4) 0.8173(3) 0.0591(13) Uani 1 1 d . . . H17A H 0.5317 1.0826 0.8166 0.071 Uiso 1 1 calc R . . C18 C 0.51161(14) 0.9176(4) 0.8549(3) 0.0598(12) Uani 1 1 d . . . H18A H 0.4917 0.9531 0.8814 0.072 Uiso 1 1 calc R . . C19 C 0.51713(13) 0.7872(4) 0.8538(3) 0.0517(11) Uani 1 1 d . . . H19A H 0.5008 0.7329 0.8793 0.062 Uiso 1 1 calc R . . C20 C 0.54696(11) 0.7367(3) 0.8148(2) 0.0365(8) Uani 1 1 d . . . C21 C 0.55429(11) 0.5993(3) 0.8081(2) 0.0377(9) Uani 1 1 d . . . C22 C 0.53093(12) 0.5061(4) 0.8356(2) 0.0473(10) Uani 1 1 d . . . H22A H 0.5094 0.5288 0.8621 0.057 Uiso 1 1 calc R . . C23 C 0.53950(13) 0.3781(4) 0.8238(3) 0.0563(12) Uani 1 1 d . . . H23A H 0.5240 0.3135 0.8425 0.068 Uiso 1 1 calc R . . C24 C 0.57059(13) 0.3476(4) 0.7847(3) 0.0540(12) Uani 1 1 d . . . H24A H 0.5766 0.2618 0.7754 0.065 Uiso 1 1 calc R . . C25 C 0.59319(12) 0.4441(3) 0.7587(2) 0.0430(9) Uani 1 1 d . . . H25A H 0.6147 0.4223 0.7320 0.052 Uiso 1 1 calc R . . C26 C 0.67279(10) 0.5906(3) 0.6301(2) 0.0330(8) Uani 1 1 d . . . H26A H 0.6623 0.6289 0.5887 0.040 Uiso 1 1 calc R . . C27 C 0.70256(11) 0.5033(4) 0.6288(2) 0.0416(9) Uani 1 1 d . . . C28 C 0.72467(14) 0.4488(4) 0.5740(3) 0.0621(13) Uani 1 1 d . . . H28A H 0.7213 0.4711 0.5251 0.075 Uiso 1 1 calc R . . C29 C 0.75133(14) 0.3622(5) 0.5944(4) 0.0772(17) Uani 1 1 d . . . H29A H 0.7664 0.3244 0.5585 0.093 Uiso 1 1 calc R . . C30 C 0.75674(13) 0.3285(4) 0.6667(4) 0.0714(16) Uani 1 1 d . . . H30A H 0.7752 0.2679 0.6784 0.086 Uiso 1 1 calc R . . C31 C 0.73597(12) 0.3811(4) 0.7211(3) 0.0559(12) Uani 1 1 d . . . H31A H 0.7398 0.3581 0.7699 0.067 Uiso 1 1 calc R . . C32 C 0.70876(11) 0.4708(3) 0.7013(2) 0.0402(9) Uani 1 1 d . . . N7 N 0.68345(9) 0.5409(3) 0.74145(18) 0.0424(8) Uani 1 1 d . . . H7B H 0.6819 0.5397 0.7885 0.051 Uiso 1 1 calc R . . P1 P 0.44115(4) 0.26697(11) 0.94057(8) 0.0550(3) Uani 1 1 d . . . P2 P 0.67786(6) 0.69978(13) 1.40943(8) 0.0823(5) Uani 1 1 d . . . F11 F 0.45707(9) 0.3650(3) 0.88209(18) 0.0858(10) Uani 1 1 d . . . F12 F 0.40113(10) 0.3250(4) 0.9250(2) 0.1129(13) Uani 1 1 d . . . F13 F 0.42358(11) 0.1738(3) 0.99917(19) 0.0993(11) Uani 1 1 d . . . F14 F 0.48108(11) 0.2070(3) 0.9526(3) 0.1153(14) Uani 1 1 d . . . F15 F 0.43398(12) 0.1642(3) 0.87939(19) 0.1054(12) Uani 1 1 d . . . F16 F 0.44819(15) 0.3676(3) 1.0017(2) 0.1301(17) Uani 1 1 d . . . F21 F 0.71347(10) 0.7750(3) 1.38047(19) 0.0909(10) Uani 1 1 d . . . F22 F 0.66381(12) 0.6955(4) 1.3276(2) 0.1144(13) Uani 1 1 d . . . F23 F 0.65740(18) 0.8280(4) 1.4197(3) 0.203(3) Uani 1 1 d . . . F24 F 0.69823(13) 0.5671(3) 1.3918(2) 0.1158(14) Uani 1 1 d . . . F25 F 0.64347(17) 0.6211(4) 1.4365(3) 0.189(3) Uani 1 1 d . . . F26 F 0.6951(3) 0.6964(5) 1.4853(2) 0.270(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.02813(16) 0.02534(14) 0.03784(18) -0.00027(12) 0.00148(14) 0.00026(11) N1 0.0291(17) 0.0303(14) 0.0438(19) -0.0032(13) -0.0001(14) 0.0029(12) N2 0.0316(17) 0.0275(14) 0.0409(18) 0.0011(13) 0.0023(14) -0.0006(12) N3 0.0322(17) 0.0362(15) 0.0391(18) -0.0040(13) 0.0027(14) 0.0041(13) N4 0.0312(17) 0.0330(15) 0.042(2) -0.0052(13) 0.0017(14) 0.0004(12) N5 0.0349(17) 0.0315(14) 0.0355(17) 0.0024(13) 0.0002(14) -0.0017(12) N6 0.0317(17) 0.0283(14) 0.0414(19) 0.0041(13) 0.0009(14) 0.0024(12) C1 0.037(2) 0.0387(19) 0.046(2) -0.0043(17) -0.0007(19) 0.0006(16) C2 0.056(3) 0.054(2) 0.054(3) -0.006(2) -0.013(2) -0.005(2) C3 0.064(3) 0.062(3) 0.054(3) 0.003(2) -0.020(2) 0.003(2) C4 0.064(3) 0.041(2) 0.047(3) 0.0064(19) -0.003(2) 0.005(2) C5 0.037(2) 0.0295(17) 0.046(2) 0.0017(16) 0.0002(17) 0.0059(15) C6 0.035(2) 0.0298(17) 0.047(2) 0.0008(16) 0.0027(18) 0.0015(15) C7 0.047(3) 0.039(2) 0.056(3) 0.0100(18) 0.001(2) -0.0016(18) C8 0.057(3) 0.032(2) 0.075(3) 0.005(2) 0.003(2) -0.0108(19) C9 0.043(2) 0.042(2) 0.060(3) -0.007(2) 0.000(2) -0.0130(18) C10 0.034(2) 0.0345(18) 0.044(2) -0.0050(16) 0.0049(17) -0.0013(15) C11 0.033(2) 0.0365(18) 0.044(2) -0.0061(16) 0.0038(18) 0.0010(15) C12 0.045(3) 0.051(2) 0.055(3) -0.012(2) -0.003(2) -0.0061(19) C13 0.054(3) 0.070(3) 0.049(3) -0.012(2) -0.012(2) 0.005(2) C14 0.059(3) 0.062(3) 0.040(3) 0.001(2) -0.006(2) 0.008(2) C15 0.042(2) 0.043(2) 0.042(2) 0.0009(17) 0.0030(19) 0.0055(17) C16 0.043(2) 0.0326(18) 0.070(3) -0.0039(19) 0.007(2) -0.0008(17) C17 0.050(3) 0.039(2) 0.089(4) -0.014(2) 0.009(3) 0.006(2) C18 0.051(3) 0.054(3) 0.074(3) -0.014(2) 0.018(3) 0.011(2) C19 0.045(3) 0.050(2) 0.061(3) -0.002(2) 0.017(2) -0.001(2) C20 0.031(2) 0.0402(19) 0.039(2) -0.0008(16) 0.0004(17) 0.0034(15) C21 0.033(2) 0.0395(19) 0.040(2) 0.0032(16) 0.0001(17) -0.0009(16) C22 0.039(2) 0.045(2) 0.059(3) 0.0057(19) 0.010(2) -0.0021(18) C23 0.050(3) 0.044(2) 0.075(3) 0.015(2) 0.011(2) -0.013(2) C24 0.057(3) 0.0314(19) 0.074(3) 0.0064(19) 0.005(2) -0.0027(19) C25 0.043(2) 0.0330(18) 0.053(3) 0.0021(17) 0.005(2) 0.0008(16) C26 0.033(2) 0.0331(17) 0.033(2) -0.0007(15) 0.0018(16) 0.0014(15) C27 0.031(2) 0.043(2) 0.051(3) -0.0117(18) 0.0065(18) -0.0050(16) C28 0.050(3) 0.073(3) 0.064(3) -0.027(2) 0.012(2) -0.008(2) C29 0.040(3) 0.079(3) 0.113(5) -0.046(3) 0.019(3) 0.001(2) C30 0.034(3) 0.049(3) 0.131(5) -0.027(3) -0.005(3) 0.007(2) C31 0.038(2) 0.037(2) 0.093(4) -0.005(2) -0.009(2) 0.0051(17) C32 0.030(2) 0.0322(18) 0.058(3) -0.0054(17) 0.0000(19) -0.0010(15) N7 0.044(2) 0.0403(17) 0.043(2) 0.0024(14) -0.0013(16) 0.0060(14) P1 0.0481(7) 0.0437(6) 0.0733(9) 0.0068(6) -0.0027(6) -0.0075(5) P2 0.1273(15) 0.0589(8) 0.0608(9) -0.0082(7) 0.0170(10) -0.0315(9) F11 0.073(2) 0.0727(18) 0.111(3) 0.0317(17) 0.0151(19) -0.0093(16) F12 0.057(2) 0.123(3) 0.158(4) 0.044(3) 0.015(2) 0.016(2) F13 0.130(3) 0.0734(19) 0.094(2) 0.0237(18) 0.014(2) -0.026(2) F14 0.067(2) 0.099(3) 0.180(4) 0.035(2) -0.020(3) 0.0147(19) F15 0.139(4) 0.081(2) 0.097(3) -0.0190(19) -0.009(2) -0.015(2) F16 0.223(5) 0.0647(19) 0.103(3) -0.0136(19) -0.030(3) -0.030(3) F21 0.094(3) 0.0728(19) 0.106(3) 0.0203(18) -0.016(2) -0.0158(17) F22 0.116(3) 0.114(3) 0.113(3) 0.000(2) -0.030(3) -0.004(2) F23 0.249(7) 0.068(2) 0.291(7) -0.026(3) 0.194(6) -0.021(3) F24 0.167(4) 0.0630(19) 0.117(3) 0.0159(19) -0.014(3) -0.008(2) F25 0.212(6) 0.090(3) 0.264(6) -0.019(3) 0.147(5) -0.059(3) F26 0.559(14) 0.193(5) 0.058(3) 0.024(3) -0.067(5) -0.211(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 1.968(3) . ? Ru N4 2.055(3) . ? Ru N3 2.068(3) . ? Ru N1 2.068(3) . ? Ru N5 2.080(3) . ? Ru N6 2.086(3) . ? N1 C1 1.339(5) . ? N1 C5 1.374(4) . ? N2 C10 1.349(5) . ? N2 C6 1.351(5) . ? N3 C15 1.346(5) . ? N3 C11 1.381(5) . ? N4 C16 1.353(5) . ? N4 C20 1.354(5) . ? N5 C25 1.347(4) . ? N5 C21 1.358(5) . ? N6 C26 1.321(5) . ? N6 N7 1.355(4) . ? C1 C2 1.374(6) . ? C1 H1A 0.9400 . ? C2 C3 1.374(6) . ? C2 H2A 0.9400 . ? C3 C4 1.385(6) . ? C3 H3A 0.9400 . ? C4 C5 1.378(6) . ? C4 H4A 0.9400 . ? C5 C6 1.472(5) . ? C6 C7 1.388(5) . ? C7 C8 1.377(6) . ? C7 H7A 0.9400 . ? C8 C9 1.383(6) . ? C8 H8A 0.9400 . ? C9 C10 1.386(5) . ? C9 H9A 0.9400 . ? C10 C11 1.475(5) . ? C11 C12 1.379(5) . ? C12 C13 1.379(6) . ? C12 H12A 0.9400 . ? C13 C14 1.378(7) . ? C13 H13A 0.9400 . ? C14 C15 1.380(6) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C16 C17 1.372(6) . ? C16 H16A 0.9400 . ? C17 C18 1.356(6) . ? C17 H17A 0.9400 . ? C18 C19 1.379(6) . ? C18 H18A 0.9400 . ? C19 C20 1.390(5) . ? C19 H19A 0.9400 . ? C20 C21 1.468(5) . ? C21 C22 1.381(5) . ? C22 C23 1.392(6) . ? C22 H22A 0.9400 . ? C23 C24 1.362(6) . ? C23 H23A 0.9400 . ? C24 C25 1.378(5) . ? C24 H24A 0.9400 . ? C25 H25A 0.9400 . ? C26 C27 1.402(5) . ? C26 H26A 0.9400 . ? C27 C32 1.397(6) . ? C27 C28 1.403(6) . ? C28 C29 1.367(7) . ? C28 H28A 0.9400 . ? C29 C30 1.394(8) . ? C29 H29A 0.9400 . ? C30 C31 1.363(7) . ? C30 H30A 0.9400 . ? C31 C32 1.400(5) . ? C31 H31A 0.9400 . ? C32 N7 1.379(5) . ? N7 H7B 0.8700 . ? P1 F16 1.564(3) . ? P1 F14 1.573(4) . ? P1 F12 1.579(4) . ? P1 F15 1.580(3) . ? P1 F13 1.585(3) . ? P1 F11 1.593(3) . ? P2 F26 1.529(5) . ? P2 F23 1.541(5) . ? P2 F25 1.561(4) . ? P2 F21 1.588(4) . ? P2 F22 1.590(4) . ? P2 F24 1.601(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru N4 95.24(12) . . ? N2 Ru N3 79.67(12) . . ? N4 Ru N3 88.74(12) . . ? N2 Ru N1 79.79(12) . . ? N4 Ru N1 92.85(12) . . ? N3 Ru N1 159.46(12) . . ? N2 Ru N5 173.83(12) . . ? N4 Ru N5 78.62(12) . . ? N3 Ru N5 100.59(12) . . ? N1 Ru N5 99.80(12) . . ? N2 Ru N6 91.76(11) . . ? N4 Ru N6 172.70(11) . . ? N3 Ru N6 90.48(12) . . ? N1 Ru N6 90.42(12) . . ? N5 Ru N6 94.40(11) . . ? C1 N1 C5 118.5(3) . . ? C1 N1 Ru 128.4(3) . . ? C5 N1 Ru 113.2(2) . . ? C10 N2 C6 122.5(3) . . ? C10 N2 Ru 119.0(2) . . ? C6 N2 Ru 118.3(2) . . ? C15 N3 C11 117.7(3) . . ? C15 N3 Ru 129.1(3) . . ? C11 N3 Ru 113.2(2) . . ? C16 N4 C20 117.7(3) . . ? C16 N4 Ru 126.4(3) . . ? C20 N4 Ru 115.7(2) . . ? C25 N5 C21 118.5(3) . . ? C25 N5 Ru 126.6(3) . . ? C21 N5 Ru 114.9(2) . . ? C26 N6 N7 107.0(3) . . ? C26 N6 Ru 129.6(2) . . ? N7 N6 Ru 123.3(2) . . ? N1 C1 C2 122.7(4) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 114.9(3) . . ? C4 C5 C6 124.1(3) . . ? N2 C6 C7 119.1(4) . . ? N2 C6 C5 113.5(3) . . ? C7 C6 C5 127.4(4) . . ? C8 C7 C6 119.4(4) . . ? C8 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? C7 C8 C9 120.4(4) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C8 C9 C10 119.0(4) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? N2 C10 C9 119.6(4) . . ? N2 C10 C11 113.0(3) . . ? C9 C10 C11 127.4(4) . . ? C12 C11 N3 120.8(4) . . ? C12 C11 C10 124.3(4) . . ? N3 C11 C10 115.0(3) . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 118.7(4) . . ? C13 C14 H14A 120.7 . . ? C15 C14 H14A 120.7 . . ? N3 C15 C14 123.2(4) . . ? N3 C15 H15A 118.4 . . ? C14 C15 H15A 118.4 . . ? N4 C16 C17 122.6(4) . . ? N4 C16 H16A 118.7 . . ? C17 C16 H16A 118.7 . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 119.0(4) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C18 C19 C20 119.6(4) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? N4 C20 C19 121.3(3) . . ? N4 C20 C21 115.2(3) . . ? C19 C20 C21 123.6(4) . . ? N5 C21 C22 121.2(3) . . ? N5 C21 C20 115.0(3) . . ? C22 C21 C20 123.7(4) . . ? C21 C22 C23 119.4(4) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C24 C23 C22 119.2(4) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? N5 C25 C24 122.4(4) . . ? N5 C25 H25A 118.8 . . ? C24 C25 H25A 118.8 . . ? N6 C26 C27 111.1(3) . . ? N6 C26 H26A 124.5 . . ? C27 C26 H26A 124.5 . . ? C32 C27 C26 105.2(3) . . ? C32 C27 C28 120.0(4) . . ? C26 C27 C28 134.8(4) . . ? C29 C28 C27 117.6(5) . . ? C29 C28 H28A 121.2 . . ? C27 C28 H28A 121.2 . . ? C28 C29 C30 121.8(5) . . ? C28 C29 H29A 119.1 . . ? C30 C29 H29A 119.1 . . ? C31 C30 C29 121.8(5) . . ? C31 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? C30 C31 C32 117.2(5) . . ? C30 C31 H31A 121.4 . . ? C32 C31 H31A 121.4 . . ? N7 C32 C27 106.3(3) . . ? N7 C32 C31 132.2(4) . . ? C27 C32 C31 121.5(4) . . ? N6 N7 C32 110.4(3) . . ? N6 N7 H7B 124.8 . . ? C32 N7 H7B 124.8 . . ? F16 P1 F14 91.2(3) . . ? F16 P1 F12 91.0(3) . . ? F14 P1 F12 177.5(3) . . ? F16 P1 F15 179.4(2) . . ? F14 P1 F15 88.6(2) . . ? F12 P1 F15 89.2(2) . . ? F16 P1 F13 89.2(2) . . ? F14 P1 F13 91.0(2) . . ? F12 P1 F13 90.2(2) . . ? F15 P1 F13 90.18(19) . . ? F16 P1 F11 89.8(2) . . ? F14 P1 F11 91.7(2) . . ? F12 P1 F11 87.23(19) . . ? F15 P1 F11 90.8(2) . . ? F13 P1 F11 177.2(2) . . ? F26 P2 F23 95.7(4) . . ? F26 P2 F25 90.7(4) . . ? F23 P2 F25 92.7(3) . . ? F26 P2 F21 89.8(3) . . ? F23 P2 F21 89.3(2) . . ? F25 P2 F21 177.8(2) . . ? F26 P2 F22 173.9(4) . . ? F23 P2 F22 89.5(3) . . ? F25 P2 F22 92.3(3) . . ? F21 P2 F22 87.0(2) . . ? F26 P2 F24 89.0(4) . . ? F23 P2 F24 175.3(3) . . ? F25 P2 F24 88.0(2) . . ? F21 P2 F24 89.9(2) . . ? F22 P2 F24 85.8(2) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.698 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.075 data_010902a _database_code_depnum_ccdc_archive 'CCDC 251482' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(2,2'-Bipyridine)(imidazole)(2,2':6',2''-terpyridine)- ruthenium(II)]bis(hexafluorophosphate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C10 H8 N2)(C3 H4 N2)(C15 H11 N3)Ru](P F6)2' _chemical_formula_sum 'C28 H23 F12 N7 P2 Ru' _chemical_formula_weight 848.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.191(5) _cell_length_b 13.802(5) _cell_length_c 19.068(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.049(7) _cell_angle_gamma 90.00 _cell_volume 3688(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8640 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14194 _diffrn_reflns_av_R_equivalents 0.1670 _diffrn_reflns_av_sigmaI/netI 0.2568 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6175 _reflns_number_gt 2148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms on carbon and nitrogen were calculated using appropriate riding models (AFIX 43, U(H) = 1.2 Ueq(C/N). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6175 _refine_ls_number_parameters 452 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2407 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.88085(6) 0.26818(6) 0.05142(5) 0.0566(3) Uani 1 1 d . . . N1 N 0.9389(5) 0.3527(8) 0.1324(5) 0.075(3) Uani 1 1 d . . . N2 N 0.9432(5) 0.1734(7) 0.1161(5) 0.056(3) Uani 1 1 d . . . N3 N 0.8447(6) 0.1455(8) -0.0036(5) 0.078(3) Uani 1 1 d . . . N4 N 0.7531(6) 0.2640(7) 0.0879(4) 0.070(2) Uani 1 1 d . . . N5 N 0.8017(7) 0.3686(7) -0.0151(5) 0.072(3) Uani 1 1 d . . . N6 N 1.0030(5) 0.2793(6) 0.0050(5) 0.063(2) Uani 1 1 d . . . N7 N 1.1039(8) 0.2794(7) -0.0732(5) 0.100(3) Uani 1 1 d . . . H7B H 1.1246 0.2763 -0.1132 0.120 Uiso 1 1 calc R . . C1 C 0.9342(8) 0.4529(10) 0.1398(7) 0.084(4) Uani 1 1 d . . . H1A H 0.9042 0.4885 0.1012 0.100 Uiso 1 1 calc R . . C2 C 0.9713(8) 0.5034(10) 0.2013(9) 0.096(5) Uani 1 1 d . . . H2A H 0.9606 0.5695 0.2054 0.115 Uiso 1 1 calc R . . C3 C 1.0246(10) 0.4521(14) 0.2558(7) 0.115(5) Uani 1 1 d . . . H3A H 1.0536 0.4843 0.2964 0.138 Uiso 1 1 calc R . . C4 C 1.0348(8) 0.3529(11) 0.2500(7) 0.095(4) Uani 1 1 d . . . H4A H 1.0708 0.3168 0.2858 0.115 Uiso 1 1 calc R . . C5 C 0.9886(8) 0.3097(9) 0.1880(7) 0.073(3) Uani 1 1 d . . . C6 C 0.9964(9) 0.2016(9) 0.1815(8) 0.090(5) Uani 1 1 d . . . C7 C 1.0412(8) 0.1306(16) 0.2276(6) 0.124(6) Uani 1 1 d . . . H7A H 1.0737 0.1487 0.2719 0.149 Uiso 1 1 calc R . . C8 C 1.0376(12) 0.0327(10) 0.2080(8) 0.117(6) Uani 1 1 d . . . H8A H 1.0719 -0.0129 0.2376 0.141 Uiso 1 1 calc R . . C9 C 0.9835(7) 0.0035(8) 0.1452(6) 0.073(3) Uani 1 1 d . . . H9A H 0.9767 -0.0619 0.1336 0.088 Uiso 1 1 calc R . . C10 C 0.9369(7) 0.0779(9) 0.0969(6) 0.065(3) Uani 1 1 d . . . C11 C 0.8802(8) 0.0628(10) 0.0256(6) 0.077(4) Uani 1 1 d . . . C12 C 0.8622(9) -0.0326(9) -0.0031(7) 0.092(4) Uani 1 1 d . . . H12A H 0.8873 -0.0870 0.0220 0.111 Uiso 1 1 calc R . . C13 C 0.8076(9) -0.0415(10) -0.0681(8) 0.109(5) Uani 1 1 d . . . H13A H 0.7963 -0.1021 -0.0891 0.131 Uiso 1 1 calc R . . C14 C 0.7713(8) 0.0365(11) -0.1006(7) 0.082(4) Uani 1 1 d . . . H14A H 0.7337 0.0297 -0.1448 0.098 Uiso 1 1 calc R . . C15 C 0.7870(8) 0.1359(11) -0.0705(7) 0.101(4) Uani 1 1 d . . . H15A H 0.7597 0.1898 -0.0951 0.121 Uiso 1 1 calc R . . C16 C 0.7349(8) 0.2076(8) 0.1444(6) 0.096(4) Uani 1 1 d . . . H16A H 0.7829 0.1692 0.1690 0.115 Uiso 1 1 calc R . . C17 C 0.6443(10) 0.2083(11) 0.1643(8) 0.141(6) Uani 1 1 d . . . H17A H 0.6343 0.1758 0.2052 0.169 Uiso 1 1 calc R . . C18 C 0.5696(11) 0.2567(16) 0.1241(11) 0.203(10) Uani 1 1 d . . . H18A H 0.5088 0.2535 0.1364 0.243 Uiso 1 1 calc R . . C19 C 0.5848(11) 0.3097(11) 0.0661(8) 0.122(5) Uani 1 1 d . . . H19A H 0.5340 0.3407 0.0382 0.147 Uiso 1 1 calc R . . C20 C 0.6785(9) 0.3171(10) 0.0485(9) 0.100(5) Uani 1 1 d . . . C21 C 0.7079(11) 0.3757(9) -0.0071(7) 0.087(4) Uani 1 1 d . . . C22 C 0.6476(8) 0.4344(10) -0.0484(8) 0.104(5) Uani 1 1 d . . . H22A H 0.5839 0.4358 -0.0424 0.124 Uiso 1 1 calc R . . C23 C 0.6753(13) 0.4892(11) -0.0966(8) 0.121(6) Uani 1 1 d . . . H23A H 0.6330 0.5315 -0.1233 0.145 Uiso 1 1 calc R . . C24 C 0.7695(13) 0.4829(9) -0.1071(7) 0.096(4) Uani 1 1 d . . . H24A H 0.7895 0.5181 -0.1437 0.115 Uiso 1 1 calc R . . C25 C 0.8353(9) 0.4245(8) -0.0637(7) 0.080(4) Uani 1 1 d . . . H25A H 0.8996 0.4243 -0.0682 0.096 Uiso 1 1 calc R . . C26 C 1.0079(7) 0.2660(8) -0.0641(7) 0.079(3) Uani 1 1 d . . . H26A H 0.9573 0.2506 -0.0995 0.095 Uiso 1 1 calc R . . C27 C 1.1555(9) 0.2971(9) -0.0131(7) 0.093(5) Uani 1 1 d . . . H27A H 1.2208 0.3093 -0.0051 0.111 Uiso 1 1 calc R . . C28 C 1.0962(11) 0.2944(9) 0.0368(6) 0.114(5) Uani 1 1 d . . . H28A H 1.1159 0.3018 0.0854 0.137 Uiso 1 1 calc R . . P1 P 0.3207(2) 0.2448(3) 0.22549(17) 0.0818(10) Uani 1 1 d D . . F1 F 0.3470(7) 0.2815(10) 0.1541(5) 0.260(7) Uani 1 1 d D . . F2 F 0.2186(5) 0.2484(13) 0.1894(5) 0.277(6) Uani 1 1 d D . . F3 F 0.2989(10) 0.2275(10) 0.2986(4) 0.289(7) Uani 1 1 d D . . F4 F 0.4237(6) 0.2660(15) 0.2567(6) 0.338(10) Uani 1 1 d D . . F5 F 0.3051(13) 0.3513(6) 0.2452(6) 0.268(6) Uani 1 1 d D . . F6 F 0.3231(14) 0.1379(7) 0.2074(6) 0.424(14) Uani 1 1 d D . . P2 P 0.6513(4) 0.6214(6) 0.1307(4) 0.204(3) Uani 1 1 d D . . F7 F 0.6445(12) 0.6455(18) 0.0511(6) 0.390(14) Uani 1 1 d D . . F8 F 0.5588(9) 0.6796(12) 0.1308(9) 0.351(10) Uani 1 1 d D . . F9 F 0.5800(8) 0.5366(9) 0.1142(11) 0.333(10) Uani 1 1 d D . . F10 F 0.7340(7) 0.5565(11) 0.1168(7) 0.324(9) Uani 1 1 d D . . F11 F 0.6574(10) 0.6177(19) 0.2110(5) 0.516(19) Uani 1 1 d D . . F12 F 0.7206(12) 0.7036(15) 0.1466(10) 0.479(17) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0500(5) 0.0528(6) 0.0647(6) 0.0062(6) 0.0024(3) 0.0024(6) N1 0.026(5) 0.106(9) 0.086(8) 0.036(7) -0.012(5) 0.022(5) N2 0.052(6) 0.071(8) 0.044(6) -0.009(5) 0.003(4) -0.011(5) N3 0.048(6) 0.131(10) 0.048(6) 0.017(6) -0.016(5) 0.002(6) N4 0.088(6) 0.074(7) 0.051(5) 0.012(5) 0.022(5) -0.011(6) N5 0.044(6) 0.084(8) 0.090(8) 0.025(5) 0.011(5) 0.015(5) N6 0.039(5) 0.064(6) 0.086(7) 0.007(6) 0.015(5) 0.001(5) N7 0.132(10) 0.095(8) 0.088(9) 0.008(6) 0.063(8) 0.013(8) C1 0.082(9) 0.047(9) 0.119(12) 0.039(8) 0.007(8) 0.007(7) C2 0.061(8) 0.083(11) 0.142(14) -0.043(10) 0.011(9) 0.003(8) C3 0.118(12) 0.153(17) 0.066(10) -0.021(10) -0.015(8) 0.023(12) C4 0.080(9) 0.090(12) 0.112(12) -0.024(9) 0.001(8) -0.002(9) C5 0.068(8) 0.070(10) 0.077(10) -0.021(7) 0.003(7) -0.019(7) C6 0.096(10) 0.079(12) 0.111(12) 0.057(9) 0.072(9) 0.051(8) C7 0.061(8) 0.26(2) 0.041(9) 0.046(11) -0.012(6) 0.043(11) C8 0.227(18) 0.050(10) 0.075(11) -0.011(8) 0.021(11) 0.025(10) C9 0.098(9) 0.067(9) 0.049(8) 0.000(7) -0.002(6) 0.013(7) C10 0.071(8) 0.049(8) 0.074(9) -0.004(7) 0.007(6) -0.006(6) C11 0.055(7) 0.072(10) 0.097(11) 0.004(7) -0.012(7) -0.015(7) C12 0.119(10) 0.058(10) 0.093(10) 0.007(7) -0.008(8) -0.023(8) C13 0.120(11) 0.065(11) 0.123(13) -0.034(9) -0.043(9) 0.001(8) C14 0.086(9) 0.073(11) 0.079(10) -0.008(8) -0.011(7) 0.008(8) C15 0.097(10) 0.124(14) 0.084(11) -0.002(9) 0.019(8) -0.042(9) C16 0.108(10) 0.090(11) 0.099(10) 0.007(7) 0.042(8) -0.042(8) C17 0.087(10) 0.178(17) 0.175(15) 0.042(11) 0.073(11) 0.003(11) C18 0.077(11) 0.27(3) 0.28(2) 0.13(2) 0.056(14) 0.031(14) C19 0.100(13) 0.113(14) 0.156(16) -0.006(10) 0.026(11) 0.026(9) C20 0.049(8) 0.103(12) 0.138(13) -0.017(9) -0.016(8) 0.042(8) C21 0.125(13) 0.054(9) 0.067(9) 0.008(6) -0.030(9) 0.010(8) C22 0.073(10) 0.115(12) 0.107(12) 0.006(9) -0.037(8) 0.053(8) C23 0.159(16) 0.092(13) 0.086(12) 0.019(8) -0.060(12) 0.014(12) C24 0.162(14) 0.046(9) 0.071(10) 0.020(6) -0.006(11) 0.011(10) C25 0.090(10) 0.050(9) 0.106(11) 0.003(7) 0.037(8) 0.003(7) C26 0.054(7) 0.058(8) 0.125(11) 0.009(8) 0.012(7) -0.004(6) C27 0.075(9) 0.135(13) 0.069(9) -0.024(9) 0.011(8) -0.051(8) C28 0.154(13) 0.131(13) 0.063(9) -0.028(7) 0.037(9) -0.075(10) P1 0.086(2) 0.073(3) 0.081(3) -0.0039(19) -0.0060(18) 0.0006(19) F1 0.216(10) 0.353(17) 0.245(12) 0.149(12) 0.144(10) 0.072(11) F2 0.129(7) 0.45(2) 0.241(11) -0.017(14) -0.010(7) 0.025(12) F3 0.492(19) 0.335(17) 0.044(5) -0.015(8) 0.051(7) -0.117(14) F4 0.152(9) 0.61(3) 0.238(14) -0.153(18) -0.014(9) -0.035(16) F5 0.46(2) 0.106(10) 0.232(13) -0.012(8) 0.024(13) 0.020(11) F6 0.78(3) 0.113(10) 0.266(14) -0.084(9) -0.254(17) 0.152(15) P2 0.088(4) 0.316(9) 0.219(8) -0.127(6) 0.054(4) -0.057(5) F7 0.283(17) 0.76(4) 0.142(11) -0.019(16) 0.081(11) 0.17(2) F8 0.304(18) 0.41(3) 0.37(2) -0.120(17) 0.162(18) -0.121(17) F9 0.132(10) 0.284(18) 0.57(3) -0.171(18) 0.014(12) -0.001(10) F10 0.102(8) 0.56(3) 0.309(16) 0.055(17) 0.044(10) 0.110(12) F11 0.207(14) 1.21(6) 0.146(11) -0.24(2) 0.071(10) -0.18(2) F12 0.278(15) 0.74(4) 0.48(2) -0.41(3) 0.265(17) -0.33(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N2 1.916(9) . ? Ru N1 2.006(10) . ? Ru N3 2.015(11) . ? Ru N4 2.042(8) . ? Ru N6 2.072(8) . ? Ru N5 2.085(9) . ? N1 C5 1.320(13) . ? N1 C1 1.393(12) . ? N2 C10 1.366(11) . ? N2 C6 1.408(15) . ? N3 C11 1.334(13) . ? N3 C15 1.410(12) . ? N4 C16 1.386(11) . ? N4 C20 1.404(12) . ? N5 C25 1.349(12) . ? N5 C21 1.366(14) . ? N6 C26 1.342(11) . ? N6 C28 1.382(12) . ? N7 C27 1.283(11) . ? N7 C26 1.412(11) . ? C1 C2 1.394(15) . ? C2 C3 1.381(15) . ? C3 C4 1.383(15) . ? C4 C5 1.392(13) . ? C5 C6 1.502(14) . ? C6 C7 1.401(15) . ? C7 C8 1.401(18) . ? C8 C9 1.378(15) . ? C9 C10 1.466(13) . ? C10 C11 1.482(14) . ? C11 C12 1.433(14) . ? C12 C13 1.360(14) . ? C13 C14 1.307(14) . ? C14 C15 1.490(15) . ? C16 C17 1.396(13) . ? C17 C18 1.380(18) . ? C18 C19 1.370(16) . ? C19 C20 1.426(16) . ? C20 C21 1.446(16) . ? C21 C22 1.341(14) . ? C22 C23 1.298(16) . ? C23 C24 1.386(16) . ? C24 C25 1.401(16) . ? C27 C28 1.366(13) . ? P1 F3 1.493(6) . ? P1 F2 1.504(7) . ? P1 F4 1.517(7) . ? P1 F6 1.517(8) . ? P1 F5 1.541(8) . ? P1 F1 1.551(7) . ? P2 F12 1.501(9) . ? P2 F11 1.522(8) . ? P2 F10 1.533(8) . ? P2 F8 1.539(9) . ? P2 F7 1.541(8) . ? P2 F9 1.546(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru N1 79.0(4) . . ? N2 Ru N3 79.4(4) . . ? N1 Ru N3 158.4(4) . . ? N2 Ru N4 96.1(3) . . ? N1 Ru N4 91.9(3) . . ? N3 Ru N4 89.2(3) . . ? N2 Ru N6 89.6(3) . . ? N1 Ru N6 90.9(4) . . ? N3 Ru N6 90.1(4) . . ? N4 Ru N6 174.0(4) . . ? N2 Ru N5 174.8(4) . . ? N1 Ru N5 101.5(4) . . ? N3 Ru N5 100.0(4) . . ? N4 Ru N5 78.7(4) . . ? N6 Ru N5 95.6(4) . . ? C5 N1 C1 113.2(10) . . ? C5 N1 Ru 117.4(9) . . ? C1 N1 Ru 129.4(8) . . ? C10 N2 C6 120.5(9) . . ? C10 N2 Ru 118.8(7) . . ? C6 N2 Ru 120.7(7) . . ? C11 N3 C15 115.1(11) . . ? C11 N3 Ru 117.0(8) . . ? C15 N3 Ru 127.9(9) . . ? C16 N4 C20 119.5(11) . . ? C16 N4 Ru 124.4(8) . . ? C20 N4 Ru 116.0(9) . . ? C25 N5 C21 119.4(11) . . ? C25 N5 Ru 125.7(8) . . ? C21 N5 Ru 114.9(8) . . ? C26 N6 C28 104.9(9) . . ? C26 N6 Ru 125.8(8) . . ? C28 N6 Ru 129.1(9) . . ? C27 N7 C26 109.9(10) . . ? N1 C1 C2 124.4(12) . . ? C3 C2 C1 117.8(14) . . ? C2 C3 C4 120.0(14) . . ? C3 C4 C5 116.8(13) . . ? N1 C5 C4 127.6(13) . . ? N1 C5 C6 114.7(12) . . ? C4 C5 C6 117.7(15) . . ? C7 C6 N2 119.3(14) . . ? C7 C6 C5 132.5(18) . . ? N2 C6 C5 108.1(11) . . ? C6 C7 C8 120.9(14) . . ? C9 C8 C7 120.4(13) . . ? C8 C9 C10 118.4(12) . . ? N2 C10 C9 120.3(10) . . ? N2 C10 C11 112.6(10) . . ? C9 C10 C11 127.1(11) . . ? N3 C11 C12 126.5(11) . . ? N3 C11 C10 112.1(11) . . ? C12 C11 C10 121.2(12) . . ? C13 C12 C11 118.2(11) . . ? C14 C13 C12 118.9(13) . . ? C13 C14 C15 123.5(13) . . ? N3 C15 C14 117.8(12) . . ? N4 C16 C17 120.0(12) . . ? C18 C17 C16 120.8(14) . . ? C19 C18 C17 120.1(15) . . ? C18 C19 C20 119.9(16) . . ? N4 C20 C19 119.3(15) . . ? N4 C20 C21 113.8(12) . . ? C19 C20 C21 126.9(14) . . ? C22 C21 N5 121.3(14) . . ? C22 C21 C20 122.5(15) . . ? N5 C21 C20 116.1(11) . . ? C23 C22 C21 122.1(15) . . ? C22 C23 C24 118.2(15) . . ? C23 C24 C25 121.2(14) . . ? N5 C25 C24 117.4(12) . . ? N6 C26 N7 107.7(10) . . ? N7 C27 C28 106.8(11) . . ? C27 C28 N6 110.5(10) . . ? F3 P1 F2 96.0(7) . . ? F3 P1 F4 89.6(7) . . ? F2 P1 F4 166.5(11) . . ? F3 P1 F6 94.1(8) . . ? F2 P1 F6 88.9(9) . . ? F4 P1 F6 102.9(10) . . ? F3 P1 F5 82.3(7) . . ? F2 P1 F5 85.1(8) . . ? F4 P1 F5 83.5(8) . . ? F6 P1 F5 172.7(10) . . ? F3 P1 F1 169.9(8) . . ? F2 P1 F1 86.3(6) . . ? F4 P1 F1 86.1(7) . . ? F6 P1 F1 95.8(9) . . ? F5 P1 F1 88.1(7) . . ? F12 P2 F11 83.7(10) . . ? F12 P2 F10 88.9(8) . . ? F11 P2 F10 103.3(11) . . ? F12 P2 F8 97.9(11) . . ? F11 P2 F8 86.0(9) . . ? F10 P2 F8 169.2(10) . . ? F12 P2 F7 88.5(11) . . ? F11 P2 F7 169.5(14) . . ? F10 P2 F7 83.5(8) . . ? F8 P2 F7 88.2(9) . . ? F12 P2 F9 179.9(11) . . ? F11 P2 F9 96.4(11) . . ? F10 P2 F9 91.0(9) . . ? F8 P2 F9 82.2(7) . . ? F7 P2 F9 91.5(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru N1 C5 -0.1(7) . . . . ? N3 Ru N1 C5 3.1(13) . . . . ? N4 Ru N1 C5 95.8(8) . . . . ? N6 Ru N1 C5 -89.5(8) . . . . ? N5 Ru N1 C5 174.6(7) . . . . ? N2 Ru N1 C1 -179.4(9) . . . . ? N3 Ru N1 C1 -176.2(9) . . . . ? N4 Ru N1 C1 -83.5(9) . . . . ? N6 Ru N1 C1 91.2(9) . . . . ? N5 Ru N1 C1 -4.7(9) . . . . ? N1 Ru N2 C10 180.0(8) . . . . ? N3 Ru N2 C10 1.2(7) . . . . ? N4 Ru N2 C10 89.2(7) . . . . ? N6 Ru N2 C10 -89.0(7) . . . . ? N5 Ru N2 C10 84(4) . . . . ? N1 Ru N2 C6 -1.4(7) . . . . ? N3 Ru N2 C6 179.8(8) . . . . ? N4 Ru N2 C6 -92.2(8) . . . . ? N6 Ru N2 C6 89.6(8) . . . . ? N5 Ru N2 C6 -97(4) . . . . ? N2 Ru N3 C11 -2.5(8) . . . . ? N1 Ru N3 C11 -5.7(14) . . . . ? N4 Ru N3 C11 -98.9(8) . . . . ? N6 Ru N3 C11 87.1(8) . . . . ? N5 Ru N3 C11 -177.2(8) . . . . ? N2 Ru N3 C15 178.7(9) . . . . ? N1 Ru N3 C15 175.5(8) . . . . ? N4 Ru N3 C15 82.3(9) . . . . ? N6 Ru N3 C15 -91.7(9) . . . . ? N5 Ru N3 C15 4.0(9) . . . . ? N2 Ru N4 C16 2.1(9) . . . . ? N1 Ru N4 C16 -77.0(9) . . . . ? N3 Ru N4 C16 81.4(9) . . . . ? N6 Ru N4 C16 165(3) . . . . ? N5 Ru N4 C16 -178.3(9) . . . . ? N2 Ru N4 C20 -172.8(8) . . . . ? N1 Ru N4 C20 108.0(8) . . . . ? N3 Ru N4 C20 -93.6(8) . . . . ? N6 Ru N4 C20 -10(4) . . . . ? N5 Ru N4 C20 6.7(8) . . . . ? N2 Ru N5 C25 180(100) . . . . ? N1 Ru N5 C25 85.2(10) . . . . ? N3 Ru N5 C25 -98.0(10) . . . . ? N4 Ru N5 C25 174.8(10) . . . . ? N6 Ru N5 C25 -6.9(10) . . . . ? N2 Ru N5 C21 0(5) . . . . ? N1 Ru N5 C21 -95.0(8) . . . . ? N3 Ru N5 C21 81.8(8) . . . . ? N4 Ru N5 C21 -5.4(8) . . . . ? N6 Ru N5 C21 172.9(8) . . . . ? N2 Ru N6 C26 123.9(9) . . . . ? N1 Ru N6 C26 -157.1(9) . . . . ? N3 Ru N6 C26 44.5(9) . . . . ? N4 Ru N6 C26 -39(4) . . . . ? N5 Ru N6 C26 -55.5(9) . . . . ? N2 Ru N6 C28 -51.0(10) . . . . ? N1 Ru N6 C28 28.0(10) . . . . ? N3 Ru N6 C28 -130.3(10) . . . . ? N4 Ru N6 C28 146(3) . . . . ? N5 Ru N6 C28 129.6(10) . . . . ? C5 N1 C1 C2 -4.6(15) . . . . ? Ru N1 C1 C2 174.7(8) . . . . ? N1 C1 C2 C3 6.8(18) . . . . ? C1 C2 C3 C4 -4(2) . . . . ? C2 C3 C4 C5 -0.6(19) . . . . ? C1 N1 C5 C4 -0.4(16) . . . . ? Ru N1 C5 C4 -179.8(9) . . . . ? C1 N1 C5 C6 -179.2(8) . . . . ? Ru N1 C5 C6 1.4(12) . . . . ? C3 C4 C5 N1 2.9(18) . . . . ? C3 C4 C5 C6 -178.3(11) . . . . ? C10 N2 C6 C7 -1.4(14) . . . . ? Ru N2 C6 C7 180.0(7) . . . . ? C10 N2 C6 C5 -179.0(8) . . . . ? Ru N2 C6 C5 2.4(11) . . . . ? N1 C5 C6 C7 -179.5(10) . . . . ? C4 C5 C6 C7 1.6(19) . . . . ? N1 C5 C6 N2 -2.3(13) . . . . ? C4 C5 C6 N2 178.7(9) . . . . ? N2 C6 C7 C8 3.2(17) . . . . ? C5 C6 C7 C8 -179.9(12) . . . . ? C6 C7 C8 C9 -5(2) . . . . ? C7 C8 C9 C10 5.2(19) . . . . ? C6 N2 C10 C9 1.6(14) . . . . ? Ru N2 C10 C9 -179.8(7) . . . . ? C6 N2 C10 C11 -178.5(9) . . . . ? Ru N2 C10 C11 0.1(11) . . . . ? C8 C9 C10 N2 -3.5(16) . . . . ? C8 C9 C10 C11 176.6(11) . . . . ? C15 N3 C11 C12 -2.6(16) . . . . ? Ru N3 C11 C12 178.5(9) . . . . ? C15 N3 C11 C10 -177.9(9) . . . . ? Ru N3 C11 C10 3.2(12) . . . . ? N2 C10 C11 N3 -2.2(13) . . . . ? C9 C10 C11 N3 177.8(10) . . . . ? N2 C10 C11 C12 -177.7(10) . . . . ? C9 C10 C11 C12 2.2(17) . . . . ? N3 C11 C12 C13 3.5(19) . . . . ? C10 C11 C12 C13 178.4(11) . . . . ? C11 C12 C13 C14 -2.2(19) . . . . ? C12 C13 C14 C15 1(2) . . . . ? C11 N3 C15 C14 0.7(14) . . . . ? Ru N3 C15 C14 179.5(7) . . . . ? C13 C14 C15 N3 0.3(18) . . . . ? C20 N4 C16 C17 -3.8(16) . . . . ? Ru N4 C16 C17 -178.6(9) . . . . ? N4 C16 C17 C18 7(2) . . . . ? C16 C17 C18 C19 -4(3) . . . . ? C17 C18 C19 C20 -2(3) . . . . ? C16 N4 C20 C19 -1.8(16) . . . . ? Ru N4 C20 C19 173.4(9) . . . . ? C16 N4 C20 C21 177.8(10) . . . . ? Ru N4 C20 C21 -7.0(13) . . . . ? C18 C19 C20 N4 5(2) . . . . ? C18 C19 C20 C21 -174.8(16) . . . . ? C25 N5 C21 C22 2.7(18) . . . . ? Ru N5 C21 C22 -177.1(9) . . . . ? C25 N5 C21 C20 -176.9(11) . . . . ? Ru N5 C21 C20 3.2(13) . . . . ? N4 C20 C21 C22 -177.2(11) . . . . ? C19 C20 C21 C22 2(2) . . . . ? N4 C20 C21 N5 2.4(16) . . . . ? C19 C20 C21 N5 -178.1(11) . . . . ? N5 C21 C22 C23 -2(2) . . . . ? C20 C21 C22 C23 177.6(14) . . . . ? C21 C22 C23 C24 3(2) . . . . ? C22 C23 C24 C25 -5(2) . . . . ? C21 N5 C25 C24 -4.3(17) . . . . ? Ru N5 C25 C24 175.5(8) . . . . ? C23 C24 C25 N5 5(2) . . . . ? C28 N6 C26 N7 -3.6(12) . . . . ? Ru N6 C26 N7 -179.5(6) . . . . ? C27 N7 C26 N6 1.9(14) . . . . ? C26 N7 C27 C28 0.8(15) . . . . ? N7 C27 C28 N6 -3.2(15) . . . . ? C26 N6 C28 C27 4.3(14) . . . . ? Ru N6 C28 C27 180.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.646 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.088